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DEPARTMENT OF COMMERCE 



Technologic Papers 



07 THB 



Bureau of Standards 

S. W. STRATTON, DIRECTOR 



No. 207 

manufacture and properties of steel 

plates containing zirconium 

and other elements 

BY 

GEORGE K. BURGESS, Physicist 
RAYMOND W. WOODWARD, Physicist 
Bureau of Standards 



FEBRUARY 2, 1922 




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1922 



DEPARTMENT OF COMMERCE 



Technologic Papers 



OF THE 



Bureau of Standards 

S. W. STRATTON. DIRECTOR 



No. 207 

manufacture and properties of steel 

plates containing zirconium 

and other elements 



BY 



GEORGE K. BURGESS, Physicist 
RAYMOND W. WOODWARD, Physicist 

Bureau of Standards 



FEBRUARY 2, 1922 




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MANUFACTURE AND PROPERTIES OF STEEL PLATES 
CONTAINING ZIRCONIUM AND OTHER ELEMENTS 

By George K. Burgess and Raymond W. Woodward 



ABSTRACT 

This paper describes the manufacture and certain physical properties obtained from 
steel plates produced from about 193 heats of steel containing in various combinations 
the following principal variable elements: Carbon, silicon, nickel, aluminum, 
titanium, zirconium, cerium, boron, copper, cobalt, uranium, molybdenum, chro- 
mium, and tungsten. 

None of the steels presented any difl5culties in rolling into plate except those contain- 
ing boron. Boron forms a complex eutectic, probably that of an iron-carbon-boron 
compotmd with iron, which is fusible at the temperatines ordinarily used in rolling, 
but at slightly lower temperatures steel containing boron can be rolled successfully. 

The usual mechanical and impact tests were carried out on all of the steels. It is 
shown that steel containing 0.40 to 0.50 per cent carbon, i to 1.50 per cent silicon, 
3 to 3.25 per cent nickel, and 0.60 to 0.80 manganese and deoxidized with a simple 
deoxidizer, such as aluminum, can be produced having a tensile strength of approxi- 
mately 300 000 Ibs./in.^ with excellent ductility and toughness. This type of steel is 
recommended for a structural material. 

Although the same high properties are obtained in steels of the above composition 
with the aid of additional elements, it does not appear necessary in general, to resort 
to such additions of more costly alloying elements. 



CONTENTS 

Page 

I. Introduction 124 

II. Composition of ingots 125 

III. Preparation of plates and test pieces 126 

1. Cropping and rolling of ingots 126 

(a) Description of ingots 126 

(6) Rolling data 127 

(c) Disposition of material 129 

{d) Ingots containing boron 130 

2 . Heat treatment 130 

IV. Properties of the material 132 

1. Critical ranges 132 

2. Microstructure 134 

(a) Zirconitun, titanium, aluminum 135 

(b) Other alloying elements 136 

(c) Soundness of the steels and structines of the normalized 

and heat-treated specimens 138 

3. Mechanical properties 140 

(o) Tensile tests 140 

(b) Impact tests 142 

(c) Hardness tests 146 

V. Comparison tests on similar material 147 

123 



124 Technologic Papers of the Bureau of Standards [Voi. x6 

Pago 

VI. Effect of various addition elements 150 

1. Group A — silicon steels ici 

2. Group B — ^nickel-silicon steels 151 

3. Group C — silicon-zirconium steels 152 

4. Group D — ^nickel-silicon-zirconium steels 152 

! 5. Group E — cerium steels 152 

6. Group F — copper steels 153 

7. Group G — boron steels 153 

8. Group H — ^uranium steels 153 

9. Group I — Imolybdenum steels 153 

10. Group J — nickel-chromium steels 154 

11. Group K — ^vanadium steels 154 

12. Group L — chromium-tungsten steels 154 

13. Group M — cobalt steels 154 

VII. Summary and conclusions 170 

VIII. Acknowledgments 171 

Appendix: The determination of zirconium in steel 172 

I. INTRODUCTION 

This investigation originated in the need of the ordnance 
departments of the Army and Navy for information regarding 
the effects on the balHstic properties of light armor plate of cer- 
tain chemical elements, such as zirconium, on the one hand, and 
the effects of such elements as uranium in reducing erosion in 
guns, on the other hand. The account here given relates mainly 
to the efforts to produce armor plate of various compositions. 

After conference with the representatives of the several estab- 
lishments interested, a joint program was outlined according to 
which the Bureau of Mines was to produce and analyze ingots of 
the desired compositions, the Bureau of Standards to manufac- 
ture and heat treat plates, carry out physical tests, microexami- 
nations and chemical analyses, and develop methods of chemical 
analysis when needed for the more unusual elements in steel, and 
the Navy Department was to carry out the ballistic tests. 

The most urgent problem was the determination of the effect 
of zirconium on the properties of carbon steels and of nickel- 
carbon steels, and especially to differentiate between the effects 
of zirconium and silicon. 

As the work progressed it was considered desirable to investi- 
gate the effects of other elements, and there were accordingly 
included steels containing titanium, aluminum, boron, molyb- 
denum, cerium, cobalt, chromium, vanadium, tungsten, uranium, 
and copper. 

In addition to the ingots furnished by Dr. Gillett, opportunity 
was given to examine plates of steel containing zirconium manu- 
factured by an automobile manufacturer. 



Woodward] Zircomum Stecls 125 

Although the results of the ballistic tests are not available for 
publication, an account of the mechanical properties and tests 
of this series of somewhat unusual steels is considered worthy of 
consideration. The nickel-silicon group appears to be of particular 
interest, as is also the fact brought out that zirconium does not 
appear- to confer any especially advantageous properties to types 
of steel here studied, and, in fact, behaves very much like silicon, 
although for carbon steels the data are not sufficiently complete 
to warrant conclusions. 

The investigation throws some additional light on the manner 
in which certain of the rarer elements enter into steel, and there 
were also developed new analytical methods for the determina- 
tion of zirconium in steels and of several of the unusual elements 
in the presence of each other. 

II. COMPOSITION OF INGOTS 

The chemical composition of all ingots was determined from 
drillings taken from both the top and bottom of the ingots. From 
each of these sets of drillings an analysis was made for all the 
elements occurring in the steel by Dr. Gillett and his associates 
at Ithaca. Samples were also taken from the top and bottom 
crops at the Bureau of Standards and further analysis made for 
the aluminum, titanium, and zirconium content.^ Since the exact 
determination of this combination of elements presents some diffi- 
culty, the method used at the Bureau is included in the appendix.^ 

The composition of the various ingots will be found in Tables 
II to 22, while Table i gives a list showing in which table the data 
for a given heat appears. The analytical values for carbon, silicon, 
manganese, nickel, and other alloying elements are as reported by 
Dr. Gillett. Those for aluminum, titanium, and zirconium are a 
weighted mean of the determinations made at the Bureau of 
Standards and by the Bureau of Mines. In case the top and 
bottom samples showed segregation to have occurred in the ingot 
the values for both top and bottom are given in the table. No 
determinations were made of the sulphur or phosphorus content 
except in the few cases noted, since the steels were made from 
Armco iron as a base, and it is believed that these steels will run 
below 0.035 psr cent sulphur, except 1256 and 1257, in which it 
was intentionally raised, and below 0.015 P^^ c^^it phosphorus. 

' These determinations were made under the direction of Dr. G. E. F. LundcU. 

•See also Lundell and Knowles, Jl. Ind. and Eng. Chem., 12, p. 563, 1920; The determination of 
zirconium in steel. 



126 



Technologic Papers of the Bureau of Standards [Voi. i6 



In addition all will contain about 0.04 per cent copper and proba- 
bly a small amount of cobalt, carried in by the commercial nickel, 
in the steels containing nickel. 

TABLE 1. — List Showing Tables in Which Composition and Mechanical Propertiea 

of Various Heats May be Found 



Heat 


Table 


Heat 


Table 


Heat 


Table 


Heat 


Table 


Heat 


Table 


No. 


No. 


No. 


No. 


No. 


No. 


No. 


No. 


No. 


No. 


1101 


13 


1163 


11 


1204 


12 


1243 


14 


1290 


14 


1102 


11 


1164 


11 


1205 


12 


1244 


22 


1291 


14 


1103 


13 


1165 


12 


1206 


12 


1245 


12 


1292 


14 


1104 


11 


1166 


12 


1207 


20 


1246 


12 


1293 


14 


llOS 


13 
13 


1167 
1168 


12 
12 


1208 
1209 


12 
12 


1247 
1248 


14 
14 






1106 


Comparison 
steels 


1107 


13 


1169 


12 


1210 


14 


1249 


14 


1109 

nil 


13 
14 


1170 
1171 


12 
12 


1211 
1212 


14 
14 


1250 
1251 


14 
12 








1112 


14 


1172 


12 


1213 


14 


1252 


15 


1 


14 


1113 


12 


1173 


20 


1214 


12 


1253 


15 


2 
3 

4 
5 


14 

18-21 

18 

19 


1114 


12 


1174 


12 


1215 


12 


1256 


15 


1115 


14 


1175 


14 


1216 


12 


1257 


15 


1117 


14 


1176 


14 


1217 


12 


1258 


15 


1118 


12 


1177 


22 


1218 


14 


1259 


15 


6 


18 


1119 


14 


1178 


22 


1219 


14 


1260 


IS 


7 
8 
9 

10 


14 
14 
18 

14 


1120 


12 


1180 


13 


1220 


14 


1261 


17 


1128 


12 


1181 


13 


1221 


14 


1263 


17 


1129 


12 


1182 


13 


1222 


14 


1264 


17 


1130 


12 


1183 


13 


1223 


14 


1267 


17 


11 


14-18 


1131 


14 


1184 


13 


1224 


14 


1268 


15 


12 
13 
14 
15 


19 

12 

14-21 
18-21 


1132 


14 


1185 


13 


1225 


14 


1269 


11 


1133 


14 


1186 




1226 


12 


1270 


11 


1134 


14 


1187 




1227 


12 


1271 


20 


1135 


18 


1188 




1228 


22 


1272 


15 


16 


14 


1136 


18 


1189 




1229 


22 


1273 


20 


17 
18 
19 
20 


14 
14 
19 

14 


1138 


14 


1190 




1230 


14 


1274 


17 


1144 


14 


1191 




1231 


14 


1275 


17 


1145 


14 


1192 




1232 


14 


1276 


17 


1146 


14 


1193 




1233 


14 


1277 


17 


21 


14 


1147 


12 


1194 




1234 


14 


1278 


17 


22 
23 
24 
25 


21 
20 
14 
14 


1155 


19 


1195 




1235 


14 


1279 


16 


1156 


19 


1196 




1236 


12 


1280 


16 


1157 


14 


1197 




1237 


12 


1281 


15-16 


1158 


14 


1198 




1238 


12 


1282 


16 


26 


14 


1159 


14 


1199 




1239 


12 


1283 


16 


27 
28 


14 
12 


1160 


14 


1200 




1240 


14 


1285 


16 


1161 


14 


1201 




1241 


14 


1286 


16 






1162 


14 


1202 


12 


1242 


12 


1289 


14 







III. PREPARATION OF PLATES AND TEST PIECES 

1. CROPPING AND ROLLING OF INGOTS 

The ingots after having been made at the Bureau of Mines 
Experimental Station at Ithaca, N. Y., as described in a forth- 
coming paper of the Bureau of Mines, were shipped to the Bureau 
of Standards and there rolled into plates. 

(a) DESCRIPTION OF INGOTS 

The first ingots received were plain, round ingots without hot 
tops, cast large end up, the length being about 15 inches, top 
diameter about 3K inches, and bottom diameter about 2% inches. 



WoSard] Zirconium Steels 127 

This series, embracing Nos. iioi to 11 20, naturally contained a 
large pipe or cavity at the upper end, and a top crop of about 5 
inches was necessary to remove physically unsound material. 

Bottom crops on this series (except Nos. 11 18 and 11 20) had 
been taken previous to receipt at the Bureau of Standards. No 
crops were taken on ingot Nos. 1101-1104, 1109, 11 11, and 11 14 
at the Bureau, as these ingots had been machined down on the 
ends and surface before shipment. 

Ingots from No. 1128 to 1158 were also of the same general 
dimensions and form as the previous ones, but with the addition 
of a hot top of about 2% inches diameter. Most of this top had 
been knocked off while the ingot was still hot, directly after 
stripping from the mold. The tops of these ingots were cropped 
just below the junction of the hot top with the body of the ingot, 
or slightly farther in a few cases, to insure sound material. The 
bottom crop was just sufficient to remove the rounded end of the 
ingot. 

The remainder of the ingots were square in cross section, about 
3 inches at the top and 2^ inches at the bottom. The length, 
exclusive of the hot tops, was about 21 inches. The average 
weight of these ingots was 41.5 pounds before cropping and 35 
pounds when ready to roll. The length after cropping was about 
18 inches. 

Table 2 gives a summary of the weight of ingots and crops for 
the various t3rpes of the ingots and also the percentage available 
for rolling after having been cropped. The data show remarkably 
well the advantage to be gained by the use of a hot top, the avail- 
able material without such means being about 65 per cent, while 
with a hot top the average was 84 per cent. This latter figure 
should be slightly reduced (possibly 5 per cent) to allow for a 
portion of the hot top having been knocked off at Ithaca. This 
corrected figure, however, agrees very well with similar data ob- 
tained on /^%-ton ingots and reported elsewhere,' especially when 
the small size of the ingots used in this investigation is considered. 

(b) ROLLING DATA 

The ingots were rolled in a two-high 16-inch plate mill, a photo- 
graph of which is shown in Fig. i. This mill is driven by a 
150-horsepower 2 30- volt direct-current motor and is nonre versing. 

'Steel Rails from Sink-Head aud Ordinary Rail Ingots, by George K. Burgess, Bureau of Standards 
Technologic Paper, No. 178 



128 



Technologic Papers of the Bureau of Standards ivoi. i6 



The motor speed is variable from 250 to 1000 revolutions per 
minute, which with the reduction gear gives a roll speed of 20 to 
80 revolutions per minute. For this work the roll speed was kept 
constant at the lowest value, corresponding to a peripheral velocity 
of approximately 83 feet per minute. 

The heating of the ingots was by means of a gas-fired semi- 
muffle furnace. Usually about 10 ingots were rolled at one heat- 
ing, and they were charged into the cold furnace and brought to 
temperature with the furnace. With the exception of those steels 
containing boron, which are discussed later, the furnace tempera- 
ture was maintained at from iioo to 1150° C. The ingots were 
rolled until their temperature had fallen to about 850° C. This 
temperature was checked in many cases by means of an optical 
pyrometer. The ingots were then reheated and the operation 
repeated. 

All of the ingots were first squared down to 2^ inches square in 
four passes by turning the ingot through a 90° angle at alternate 
passes. This gave a maximum reduction of about 10 per cent 
per pass. 

Ingots up to 1 163 were then cross rolled until 6 to 7 inches wide 
and then rolled lengthwise until % inch thick. The average 
size of finished plate was about 28 by 6}4 by % inch. A total of 
about 40 passes was required, with about 5 per cent reduction per 
pass. The other ingots were entirely cross rolled after squaring, 
producing plates of various sizes, usually about 20 by 13 by _J^ 
inch (or ^ inch). 

It is probable that the percentage reductions per pass could be 
considerably increased, but since the rolling properties of the 
majority of the ingots were unknown it was deemed advisable to 
have a considerable margin of safety. A portion of those ingots 
which were rolled into long narrow plates (iioi to 1162) was cut 
off and rerolled to Vi inch thickness. 



TABLE 2 


. — ^Average Ingot 


Weights 






Ingot Nos. 


Original 
weight 


Top crop 


Bottom 
crop 


Cropped 
ingot 


Available 
for rolling 


Loss in 
rolling 


1101-1120 


Pounds 
34.5 
34.5 
41.5 
40.5 


Pounds 

12.0 

5.9 

4.8 

5.3 


Pounds 


Pounds 
21.2 
27.1 
35.0 
32.7 


Per cent 
64.9 
79.8 
84.2 
82.4 


Per cent 
3.1 


1128-1158 


1.5 
1.8 
1.7 


2.3 


1159-1293 


1.9 


Average ol all 


2.0 







Burgess l 
Woodwardj 



Zirconium Steels 



129 



(c) DISPOSITION OF MATERIAL 

The plates from ingots iioi to 1162 were sawed similar to 
sketch of Fig. 2, which represents plate No. 1 129, although typical 
of all. AB and GF were plates for ballistic tests, BC and CD 



8f 



1129 



^ 



I If 



Fig. 2. — Disposition of material from plates rolled from small ingots 

each about i inch wide, were for tensile specimens, EF for micro- 
scopic examination and thermal analyses, while the remaining 
small piec'^s were held in reserve. The lengths of the two plates 
were so adjusted that the rerolled portion would be the same 
length as the unrolled portion. 




Fig. 3. — Disposition of material from plates rolled from large ingots 

From the later plates (i 163 to 1293) a single balHstic test piece 
was cut 12 by 12 inches, or as large as possible, if the ingot was too 
small to permit of this dimension. The other test pieces were 
taken then as shown by the typical diagram for plate No. 11 73 
in Fig. 3. yl is the ballistic plate, B and C tensile specimens, 



130 Technologic Papers of the Bureau of Standards ivoi. 16 

D for impact sample, and E and F for microscopic examination 
and thermal analyses, respectively. Any plates which were not 
perfectly fiat were straightened at a temperature of about 800° C 
by means of a hydraulic forging press. The plates were not 
pickled until after heat treatment. 

(d) INGOTS CONTAINING BORON 

As was anticipated, considerable difficulty was experienced in 
rolling the ingots containing even small percentages of boron. 
Ingots Nos. 1254 (0.73 per cent B) and 1255 (0.30 per cent B) 
were heated in the ordinary manner to 1100° C preparatory to 
rolling. Upon removing these ingots from the furnace with tongs 
they fell apart under their own overhanging weight, furnishing a 
striking example of hot-shortness. No. 1262, containing 0.46 
per cent boron, was heated to only 960° C and Hkewise broke after 
partial rolling. Nos. 1261, 1263, and 1264 were similaj"ly heated 
and were rolled satisfactorily, although containing 0.71, 0.23, and 
0.46 per cent boron, respectively. Nos. 1265 and 1266 were par- 
tially rolled, but broke up under the rolls and, in fact, were so hard 
to roll that two of the coupling collars of the mill were also broken 
at the same time. These ingots contained 0.23 and 0.46 per cent 
boron, respectively. 

No difficulty was encountered in rolling Nos. 1267 (0.44 per 
cent B), 1274, 1275, 1276, 1277, and 1278 (all containing o.io 
per cent B) , although Nos. 1274 and 1276 showed numerous cracks 
and fissures in the finished plates. 

2. HEAT TREATMENT 

In determining the mechanical properties of the series of steel 
two needs were considered. First, it was desirable to correlate the 
mechanical properties of the steels with their balHstic properties; 
and, second, the large number of steels of varying composition 
made available an opportunity for studying the effect of some of 
the more uncommon alloying elements on the properties of steel. 
To satisfy properly the first requirement, tensile and impact speci- 
mens should be prepared from the heat-treated plates. This, 
however, because of the hardness of the plates, was practically 
impossible to carry out without what seemed to be unwarranted 
expense and time. For the second requirement it would be pref- 
erable to make tests on a series of specimens from each composi- 
tion drawn back to various temperatures after quenching from 
the proper temperature. This, again, would have required con- 



Burgess T 
Wood-ivardi 



Zirconium Steels 



131 



siderable additional work; and, moreover, there was not enough 
material to make a complete survey of the entire tempering 
range. 

A compromise was accordingly effected whereby tensile tests 
were made on normalized and heat-treated specimens cut from the 
plates before heat treatment, as noted in Section III, i (c) . The 
heat treatments were similar for all compositions of the series. 
That is, after normalizing and quenching in oil each from a tem- 
perature 30° C above the end of the upper critical range the speci- 
mens were drawn back at a temperature 175° C for three hours, 
this being the same treatment given the plates for ballistic testing. 

TABLE 3. — Nonnalizing and Hardening Temperatures 
[All temperatures in ° C] 



No. 


Temp. 


No. 


Temp. 


No. 


Temp. 


No. 


Temp. 


No. 


Temp. 


1101 


840 


1159 


780 


1195 


840 


1231 


800 


1271 


780 


1102 


860 


1160 


780 


1196 


860 


1232 


780 


1272 


820 


1103 


825 


1161 


840 


1197 


860 


1233 


780 


1273 


820 


1104 


840 


1162 


780 


1198 


900 


1234 


840 


1274 


820 


1105 


810 


1163 


860 


1199 


900 


1235 


860 


1275 


840 


1106 


860 


1164 


860 


1200 


820 


1236 


840 


1276 


760 


1107 


860 


1165 


820 


1201 


840 


1237 


840 


1277 


800 


1109 


800 


1166 


860 


1202 


860 


1238 


800 


1278 


850 


nil 


770 


1167 


780 


1204 


840 


1239 


800 


1279 


750 


1112 


790 


1168 


840 


1205 


820 


1240 


800 


1280 


780 


1113 


770 


1169 


820 


1206 


820 


1241 


780 


1281 


780 


U14 


770 


1170 


780 


1207 


800 


1242 


800 


1282 


800 


1115 


780 


1171 


860 


1208 


800 


1243 


800 


1283 


780 


1117 


800 


1172 


860 


1209 


800 


1244 


820 


1285 


820 


1118 


785 


1173 


840 


1210 


860 


1245 


820 


1286 


800 


1119 


810 


1174 


840 


1211 


860 


1246 


800 


1289 


800 


1120 


820 


1175 


840 


1212 


800 


1247 


840 


1290 


820 


1128 


820 


1176 


820 


1213 


800 


1248 


880 


1291 


780 


1129 


840 


1177 


860 


1214 


820 


1249 


800 


1292 


780 


1130 


820 


1178 


860 


1215 


800 


1250 


920 


1293 


800 


1131 


830 


1180 


860 


1216 


820 


1251 


820 






1132 


830 


1181 


860 


1217 


800 


1252 


800 






1133 


820 


1182 


860 


1218 


820 


1253 


805 






1134 


820 


1183 


860 


1219 


820 


1256 


840 






1135 


780 


1184 


900 


1220 


800 


1257 


840 






1136 


780 


1185 


900 


1221 


820 


1258 


780 






1138 


805 


1186 


900 


1222 


780 


1259 


780 






1144 


820 


1187 


900 


1223 


780 


1260 


820 






1145 


820 


1188 


900 


1224 


820 


1261 


880 






1146 


780 


1189 


900 


1225 


820 


1263 


880 






1147 


790 


1190 


860 


1226 


840 


1264 


820 






1155 


805 


1191 


860 


1227 


840 


1267 


880 






1156 


805 


1192 


860 


1228 


800 


1268 


840 






1157 


810 


1193 


860 


1229 


820 


1269 


840 






1158 


780 


1194 


840 


1230 


760 


1270 


840 







The normalizing and hardening treatments for the small- 
test specimens were carried out in a small electric muffle fur- 
nace; the specimens were placed in the cold furnace, brought 
to the desired temperature with the furnace, and held at that 
temperature for 15 minutes. The normalized specimens were 



i;32 Technologic Papers of the Bureau of Standards Woi. i6 

allowed to cool in the air, and the specimens to be hardened 
were quenched in the oil at room temperature. In Table 3 
are given the common normalizing and quenching tempera- 
tures. For tempering, the specimens were heated in an oil 
bath to 175° for three hours and allowed to cool in the air 
after removing from the bath. 

The duplicate tensile specimens from each plate were, in 
general, normalized at the same time, and then one of them 
hardened and tempered and the other kept in the normalized 
condition. 

The ballistic plates were heat treated in a manner similar 
to that used for the test specimens, except that larger furnace 
units were required and the plates were held at the desired 
temperatures for 45 minutes before withdrawing from the 
furnace. 

IV. PROPERTIES OF THE MATERIAL 
1. CRITICAL RANGES 

In order to prescribe properly the heat treatment of the 
various steels, the critical ranges of several of them were deter- 
mined, particularly those containing the more unusual elements, 
such as zirconium, boron, cerium, copper, and large amounts 
of silicon. Inverse rate curves were obtained on samples of 
1.5 to 2.0 grams mass by means of a modified Rosenhain fur- 
nace.* 

The temperature measurements were taken with a platinum, 
90-platinum lo-rhodium thermocouple. The rate of heating 
and cooling was approximately 0.20° C per second, while the 
maximum temperature to which the specimen was carried 
varied between 840 and 920° C. 

Table 4 gives the results obtained, together with the com- 
position of the materials investigated. Although the end of 
the AC2-3 transformation is all that is needed to determine 
the proper heat treatment, the other values are included as a 
matter of interest. For comparison there are also shown in 
the table data for a plain carbon and a 3 per cent nickel steel, 
both of which contain the other elements within commercial 
limits. 

* Scott and Freeman, Bull. Am. Inst, of Min. and Met. Eng., No. 152, p. 1429; August, 1919. Also Bu- 
reau of Standards Scientific Paper, No. 348. 



Burgess I 
Woodwardj 



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1 34 Technologic Papers of the Bureau of Standards Woi. i6 

By comparing C 24, 1104, and 1102, containing, respectively, 
0.22, 0.66, and 1. 1 5 per cent silicon, it will be noticed that silicon 
progressively raises the Ac ranges and the Arg.j range. The Ari 
point is also raised, but not to so great an extent as the other 
values. This effect is also the same in the presence of nickel, as 
shown by Nos. iiii and 11 12. 

Zirconium has about the same effect on the critical ranges as 
silicon, as will be observed from an inspection of the several data. 

The efifect of cerium is apparently rather small and irregular, as 
will be seen from Nos. C24 and 1272. The Ac^ and Ax^ points are 
raised somewhat and the AC2-3 ^^^ -^^^3-2 points decreased by about 
a similar amount. 

Copper evidently produces the same result upon the critical 
ranges as an equal amount of nickel. No. 1279 having values that 
would be expected for a 3 per cent nickel steel with 0.58 per cent 
carbon. 

In specimen No. 1 135, containing 0.78 per cent of molybdenum, 
the Aci range is about normal for a steel of similar composition but 
without the molybdenum, whereas the Ar^ range has been consid- 
erably depressed, as has also been observed by other investigators. 

From Nos. 1255, 1262, and 1264, containing boron in amounts 
from 0.06 to 0.49 per cent, and by comparison with Nos. C 24 and 
1 133, keeping in mind the variations in composition, it appears 
that boron raises all of the ranges somewhat. 

2. MICROSTRUCTURE 

(By S. Epstein) 

It must be assumed that if zirconium or any of the other elements 
that were used are to have any virtue as additions to light armor- 
plate steels they should exert some noticeable effect on the micro- 
structure of these steels at least in some stage of the heat-treated 
state, if not in the annealed condition. Also, if any true com- 
parisons are to be drawn between steels of different chemical com- 
positions from tests of their mechanical properties, it is plainly 
essential to know that the tested specimens have all been treated 
alike, or, if there are differences in the treatments, to know where 
they occur. It was the object, therefore, in the microscopic 
examination first to determine the role played by the zirconium, 
as well as the other addition elements in the steels, and, second, to 
examine the plates and test specimens for variations in soundness 
and heat treatment. 



wZward] Zirconium Steels 135 

(a) ZIRCONIUM, TITANIUM, ALUMINUM 

A steel containing zirconium can at once be recognized under the 
microscope by the presence of bright-yellow square inclusions not 
plainly visible at magnifications lower than 500 diameters (see 
Fig. 4) . They are not affected by the ordinary alcoholic nitric or 
picric acid etching solutions, but retain their lustrous yellow color. 
In the steels examined these yellow inclusions were generally asso- 
ciated with orange-pink square inclusions and irregularly shaped 
purplish-gray ones. By a comparison of the chemical composi- 
tions of the steels the orange-pink ones were traced to the presence 
of titanium, while the piu-lpish-gray ones are probably due to 
alumium. However, this last point could not be established as 
positively as with the yellow and orange-pink inclusions (see Fig. 5) . 
All of the inclusions manifested a tendency to form groups of tiny 
segregates, which when rolled, flattened out to thin plate-like 
streaks (see Fig. 6) . These plates could readily be seen with the 
naked eye in the polished and etched specimens as yellow streaks. 
They could be noticed, also, in the fractures of some of the tested 
tension bars and impact specimens as laminations. In the speci- 
mens containing zirconium and titanium in which cracks were 
found the inclusions were most numerous very close to the cracks. 
Very few of the inclusions were found outside the segregates and 
streaks or away from the cracks. 

Except for the bright-yellow square inclusions, which persisted 
throughout the working of the steel, the presence of zirconium 
was not found to affect the microstructure of the steels in any 
respect. Although the steels examined were regarded for the 
most part as alloy steels, the majority of the series under the 
microscope looked like plain carbon steels (see Fig. 7). In the 
air-cooled specimens it was considered that if any martensite 
or troostite were found it must be attributed to a seff-harden- 
ing property or retardation of the Ax^ transformation produced 
by the alloying elements. Otherwise, the structure would con- 
sist of granular pearlite and sorbite. Many of the other steels, 
to be referred to later (see Fig. 8), did show some martensite 
and troostite in the normalized specimens; but in no case was 
the presence of martensite or troostite in air-cooled specimens 
found to be due to zirconium. It may be that not all of the 
zirconium goes to form the characteristic yellow squares and 
that some of it goes into solution in the steel; but in that case it 
does not have a marked effect on the microstructure. In this 



136 Technologic Papers of the Bureau of Standards iVoi.i^ 

respect it may be likened to silicon, which goes into solution but 
the presence of wlaich in small amounts can not be detected under 
the microscope. Thermal analyses seem to indicate that part at 
least goes into solution. Titanium and aluminum also formed 
characteristic inclusions, but otherwise gave no sign of their pres- 
ence under the microscope. 

The yellow square inclusions are very hard, but because they 
make up such a small proportion of the mass of the steel it can 
scarcely be conceived that they can exert a very great influence 
on its mechanical properties. The fact that they are associated 
in the form of segregates is a disadvantage, especially in an armor- 
plate steel. Wherever cracks were found in steels containing zir- 
conium the yellow inclusions were most numerous near the cracks, 
and the conclusion that the cracks are in some way associated with 
the plates of inclusions appears to be warranted. The yellow 
inclusions of zirconium are very similar to the orange-pink ones 
of titaniinn, and with regard to the tendency of the former to 
segregate and form its negative effect on the microstructure it may 
also be compared to titanium, which is regarded as a scavenger 
and not a true alloying element. In general, zirconium, titanium, 
and aluminum may all be put in one class. They appear to act 
primarily as scavengers, and when they are not removed as part 
of the slag are present in the steel in the form of inclusions. They 
may go into solution in the steel, but in that case their presence 
can not be detected in the microscope and their effect would 
appear to be slight or negligible. In the form of inclusions they 
can not do much good, and if these are segregated and rolled out 
into thin plate-like streaks they may be detrimental. 

(b) OTHER ALLOYING ELEMENTS 

In contrast to zirconium, titanium, and aluminum, the other 
additions to the steels may be regarded as true alloying elements. 
Carbon, silicon, manganese, and nickel were not considered as 
special additions in this respect, and while their presence in the 
course of the examination was always noted they were not under 
particular observation. The other alloying elements may be 
grouped as follows: (i) Chromium, tungsten, vanadium, molyb- 
denum; (2) cerium, uranium ; (3) copper; (4) boron. 

The first four — chromium, tungsten, vanadium, and molyb- 
denum — go into solution and produce a martensitic pattern in 
the air-cooled specimens (see Fig. 8, a, b, c, d). Cerium and 
uranium go into solution and produce a martensitic pattern in the 



Bureau of Standards Technologic Papers, Vol. 16 




/ 




N 



-^ 



/ 



Fig. 4. — Inclusions in ingot nog as cast containing o.ii per cent zirconium. 
Etching, 2 per cent nitric acid 

(a) The bright yellow inchisions can not be distinguished at this magnification. Xioo 

(6) This spot shows the average number of inclusions which are indicated by the arrows. 

They are bright yellow in color. Xsoo 
(c) A segregate of the bright yellow square inclusions is here shown, ilost of these inclusions 

are segregated in this way. X 500 



Bureau of Standards Technologic Papers, Vol. 16 




H# 



y* 




> 




Fig. 5. — Different types 
the steels. Not etched. 



C 

of inclusions found ii 
Magnification X500 



(a) Steel 115S. Al, 0.173 Per cent; Ti, 0.028 per cent; Zr, 
0.22 per cent. Of the square inclusions some are bright 
yellow and some are orange-pink. The yellow inclusions 
are due to zirconium, the orange-pink to titanium. The 
circular inclusions arranged in a threadlike continuity are 
purplish gray in color and may be due to aluminum 

(b) Steel 1176. Al, 0.25 per cent; Ti, 0.09 per cent; Zr, 
O.I I per cent. A threadlike streak of the gray similar to (0) 
is to be seen. In the cluster of square inclusions indicated 
by the arrow the larger light-colored ones are bright yellow, 
the smaller darker ones are orange-pink 

(c) Steel 1213. Ti, 0.04 per cent; Zr, 0.34 per cent. _ This 
shows a segregate of small yellow and orange-pink- inclu- 
sions. Most of these inclusions are found in these segregates, 
very few outside 



Bureau of Standards Technologic Papers, Vol. 16 




Fig. 6. — Segregates of Ti and Zr inclusions rolled out into 

tin plate-like streaks 

Steel I2II. Butt— Ti, 0.07 per cent; Zr, 0.77 per cent. Top — Ti, 0.06 
per cent; Zr, 0.92 per cent. The thin plates appear as yellow streaks 
easily visible to the naked eye in the polished and etched specimens. 
In the fractures of the impact and tension bars they look like lami- 
nations. Not etched. X2 



Bureau of Standards Technologic Papers, Vol. 16 


















i^■^ 



Fig. 7. — Micro structure of air-cooled speci- 
mens of steel containing Ti and Zr. 
Etching, 2 per cent nitric acid; magnifi- 
cation, X500 

(a) Steel 1185. C, 0.26 per cent; Ni, — ; Al, 
0.021 per cent; Zr, 0.30 per cent. The structure 
is granular pearlite and ferrite 

(fc) Steel 1186. C, 0.26 per cent; Ni, 2 per cent; 
Al, 0.013 per cent; Ti, 0.04 per cent; Zr. 0.24 per 
cent. The structure is again granular pearlite 
and ferrite. The structure is not essentially- 
different from that of a steel containing a 
similar percentage of nickel but no other 
additions 

(c) Steel 1225. C, 0.27 per cent; Ni, 3.04 per 
cent; Ti, 0.22 per cent; Zr, .034 per cent. The 
structure is granular pearlite and ferrite. In 
no case was the presence of Ti or Zr found to 
produce a martensitic pattern 



Bureau of Standards Technologic Papers, Vol. 16 









p:®*:^*'-:'^: 



_^^,j^,^.,^,^ 





1? 



1-^ 




Fig. 8. — Microstructure of air-cooled spechnens containing other alloying elements. 
Etching, 2 per cent nitric acid; magnification, XS^o 

(a) Steel 1155. C, 0.38 per cent; Ni, 3.60 per cent; Cr, 1.14 per cent. The angular structure is typical 

of air-cooled nickel chromium steels 
(6) Steel 1178. C, 0.32 per cent; Ni, 3.5 per cent; Cr, 2 per cent; W, 0.90 per cent. The angular 

structure is characteristic 

(c) Steel 1207. C, 0.60 per cent; Ni, 3.6 per cent; Vd, 32 per cent 

(d) Steel 1135. C, 0.41 per cent; Ni, 3.5 per cent; Mo, 0.78 per cent 

(e) Steel 1258. C, 0.39 per cent; Ni, 2.65 per cent; Ce, 1.35 per cent. This steel displays a character- 
istic martensitic structure, due doubtless to the presence of the cerium 

(/) Steel 1228. C, 0.63 per cent; Ni, 3.01 per cent; N, 0.52 per cent. The uranium has produced a 

martensitic pattern 
(g) Steeli226. C, 0.40 per cent; Si i. 61 per cent; M, 0.90 per cent; Ni, 3.04 per cent. The combination 

of high Si. Mn, and Ni has resulted in a martensitic pattern 
(A) Steel 1282. C, 0.45 per cent; Si, i.io per cent; Mn, 0.84 per cent; Ni, 1.92 per cent; Cu, 1.35 per 

cent. The high percentage of copper had produced some martensite 



Bureau of Standards Technologic Papers, Vol. 16 

















Fig. g. — Inclusions in cerium, and uranium 
steels. Etching, 2 per cent nitric acid 

(o) Steel I2S2. Air-cooled, Ce, 0.55 per cent. A large 
number of inclusions were segregated in streaks in this 
specimen. These streaks could be plainly seen with the 
naked eye. The shape and color of the inclusions can 
not be distinguished at the magnification of this micro- 
graph, but at 500 diameters most of them appear as cir- 
cular gray inclusions, while some are orange with gray 
markings inside the circumferences. The latter in- 
clusions were found only in the cerium steels. X 50 

(6) Steel 1228. Air-cooled uranium, 0.52 per cent. A 
large number of inclusions were segregated in this spot, 
together with the long slag inclusion shown here. At 
higher magnification it can be seen that the inclusions 
are circular and of a deep blue color. The typical 
angular structure resulting from the presence of uranium 
is especially noticeable in this segregated area. X 100 



Bureau of Standards Technologic Papers, Vol. 16 




^.. 




"'■^■".i ' ■-■;'■/ •'•/■• -■''" '"^'■''^^{l^^^^iiJ'y ('•'■'.' A ' ■ *' 






.^-.^ ■ 



^ 



;% «." 



':^^'-^c.--"'f:^ 















c 

Fig. io. — Characteristic structure of boron steel 

(a) Steel 1262, containing 0.49 per cent B, which broke in 
the rolls. This shows the eutectic network. Not etched. 
Xioo 

(6) The eutectic etches dark with sodium picrate. This 
also shows where some of the eutectic has coalesced into 
the circular particles. Etching, sodium picrate, X500 

(c) The eutectic is fusible at the temperature ordinarily 
used in rolling. The cracks in the broken ingot all fol- 
lowed the network of the eutectic. This micrograph 
shows where a larger mass of eutectic has located a crack. 
Etching, sodium picrate. Xso 



Bureau of Standards Technologic Papers, Vol. 16 



\ 



/"> 








5 ;V 



• i 



* » 



% 



'^>-.'.. 












■■^'-r-ii'.l 



Fig. II. — Rolled and heat-treated steels containing boron, X500 

(a) Steel 1275. B, 0.08 per cent. This shows particles of the boron compound in the rolled and 

normalized specimen. Etching, sodium picrate 
(6) Same steel as (a). This shows the particles of the boron compound in the quenched specimen. 

Etching, sodimn picrate 

(c) Steel 126;. B, 0.30 per cent. This is the air-cooled specimen. The white sharply outlined 
particles are the boron compound. Etching, 2 per cent nitric acid 

(d] Same steel as (c), quenched. There are no definite circular and elongated particles, but a 
eutectic structure is present. This may be due to the fact that the specimen was quenched 
from a temperature high enough to allow the eutectic to form again. Etching, 2 per cent nitric 
acid 



■wwviw^w^mf^pp 



Bureau of Standards Technologic Papers, Vol. 16 





//Sg 



/.Z/3 



U 



/-e/^ 




Fig. 12. — Types of flaws existing in some of the steels. 
Etching, 2 per cent nitric acid 



(a) Steel 113S, H. T., cracked. Steel 1213, H. T., yellow streaks 
of titanium and zirconium inclusions. Steel 1215, H. T., 
dendritic. These specimens were taken from the shoulders of 
the tension bars. In the other steels that showed cracks the 
cracks were about the same size as in 1158, but there were not 
as many, generally one or two. X i 

(6) This shows the dendrites in Steel 1215, H. T., at higher magni- 
fication. X 50 



Bureau of Standards Technologic Papers, Vol, 16 





h 

Fig. 13. — Influence of considerable 
amounts of ferrite on tensile properties 
of heat-treated specimens, Y^^o 

{a) Steel 1144. C, 0.38 per cent; Si, 1.3s per 
cent; Mn, 0.84 per cent; Ni, 3.10 per cent; Al, 
0.005 per cent; Ti, 0.017 per cent; Zr, 0.32 per 
cent. This steel gave 307 000 lb,/in.2 tensile 
strength with 7.5 per cent elongation in 2 
inches, and 21.7 per cent, reduction in area in 
the heat-treated bar. The structure is fine 
martensite 

(6) Steel 1197. C, 0.32 per cent; Si, 1.37 per 
cent; Mn, 0.60 per cent; Ni, 3.05 per cent; Al, 
0.02 per cent; Ti, 0.17 per cent; Zr, 0.32 per 
cent. This steel is of almost identical chemi- 
cal composition as one shown in (a), but gave 
only 217 000 lb.,/in.2 tensile strength with 3 
per cent elongation in 2 inches and 27.5 per 
cent reduction in area. The carbon is slightly 
lower and may partly account for the large 
amount of f errite shown in the micrograph , but 
it is more probable that this is, because the 
specimen was not heated high enough before 
quenching 



wZward\ Zirconium Steels ^ 137 

air-cooled specimens (see Fig. 8,e,f), but the steels also show char- 
acteristic inclusions. At a magnification of 500 diameters the 
two cerium steels that were examined were found to contain a 
large number of gray inclusions, and also some large circular 
orange inclusions, with interior light-gray markings. The ura- 
nium steels contained deep-blue inclusions (see Fig. 9) . It seems 
that cerium and uranium, in a way somewhat similar to manganese 
(see Fig. S,g), act both as true alloying elements and to produce 
soundness in the metal. Copper goes into solution, but did not 
produce a martensitic pattern in the air-cooled specimens, except 
in the one of high copper content, i .35 per cent (see Fig. S, h). 

Boron forms a complex eutectic, probably that of an iron- 
carbon -boron compound with iron (see Fig. 10). The difficulty 
experienced in rolling the ingots containing boron is due to the 
fusibility of this eutectic at the temperatures ordinarily used for 
rolling. In the ingots that broke in the rolls the cracks in the 
polished specimens were found to follow the eutectic structure 
observed in the steels as cast, but in other places no traces were 
visible. Instead hard spherical particles, evidently of a single 
constituent of the same appearance as iron carbide, were found 
(see Fig. 11, a, b). The mechanical working probably breaks up 
the eutectic, the iron of the eutectic is absorbed by the iron of the 
matrix, while the iron-boron-carbon compound coalesces into the 
hard circular particles. These particles no longer form a weak 
brittle network and may have an appreciable hardening effect on 
the properties of the steel which may be desirable for the piurpose 
of armor plate. Care must be taken, however, in the final heat 
treatment that the steel is not heated to too high a temperature 
before quenching, as the eutectic will then again appear and render 
the steel unsuitable (see Fig. 11, d). In the unetched state both 
the eutectic and the hard circular particles are pink, they both 
etch dark with sodium picrate, similar to simple iron carbide, and 
are not etched by 2 per cent nitric-acid etching, but appear white 
in contrast to the etched matrix (compare Fig. 11, a, b with Fig. 
II, c). 

All of the above elements are true alloying additions; they are 
metallic constituents of the finished steel. The properties they 
confer upon the steel can not be established from a microscopic 
examination alone, but must be determined by physical tests. 
In the light of the considerations indicated above, however, they 
may all give good results, but more care perhaps must be taken 

63593°— 22 2 



138 Technologic Papers of the Bureau of Standards [Voi.i6 

in the making and treatment of the cerium, uranium, and boron 
steels than of the others. 

(c) SOUNDNESS OF THE STEELS AND STRUCTURES OF THE NORMALIZED AND 

HEAT-TREATED SPECIMENS 

Not all the steels that were made up were examined under the 
microscope. Typical specimens, however, were chosen from every 
class of chemical composition, and all those specimens that gave 
exceptional or unexpected values in the tension tests were exam- 
ined. Some samples were examined from the ingot as cast and 
some from the plates as rolled, but the great majority of the 
specimens were taken from the tested tension bars. 

In most of the steels that contained zirconium and titanium in 
appreciable amounts there were found in the polished and etched 
specimens the thin, yellow streaks which are the segregates of 
the zirconium and titanium inclusions rolled out into plates (see 
Fig. 12, a, steel 12 13). Many of the steels also showed small 
longitudinal cracks in the specimens (see Fig. 12, a, steel 1158), 
while in others there appeared a pronounced dendritic pattern 
(see Fig. 12, a, steel 12 15, and Fig. 12, h). These features are of 
sufficient size as to be seen with the naked eye. The streaks and , 
cracks, since they occur longitudinally in the specimens, should 
not be expected to have much effect in lowering the tensile prop- 
erties as measured. The dendritic pattern, which of itself is con- 
sidered undesirable, was not found to be associated particularly 
with steels that gave low values in tension. In fact, some of the 
steels which had the highest tensile properties showed a dendritic 
pattern. This is perhaps because these steels were rolled with the 
least number of reheatings, giving a better plate by avoiding 
repeated heatings and oxidation. The steels that were rolled in 
the latter part of the investigation, presumably most expertly, 
gave the largest percentage of dendritic structures. 

The following is a list of these steels which showed small cracks 
in the specimens examined (see Fig. 12) and those which had a 
dendritic structure. The normalized steels are marked N. and the 
heat-treated ones H. T. : 

Dendritic : 

1103, N. and H. T. 
1 132, N. and H. T. 

"35. N. 
1136, N. 

1167, N. ^ 

1168, N. and H. T. 



Cracked : 








1 106, 


N. 






1107, 


N. 






1109, 


N. 






1119, 


N. 






"57. 


H. 


T. 




1158, 


N. 


andH. 


T. 



Burgess "I 
Woodwardj 



Zirconium Steels 



139 



Cracked— 
1176, 
1178, 
1 189, 
1211, 
1213, 
isaS, 
1229, 
1236, 

1237. 
1258, 
1274, 

"75. 
1278, 
1286, 



-Continued 

H. T. 

N. 

H. T 

H. T. 

N. 

N. and H. T. 

H. T. 

N. and H. T. 

H. T. 

N. and H. T. 

N. and H. T. 

N. 

N. and H. T. 

N. 



Dendritic — Continued 

1190, N. 
1200, N. 

1205, N. 

1206, N. 

1207, N. and H. T. 

1215, N. and H. T. 

1216, N. 

1219, N. and H. T. 

1224, N. 

1227, N. and H. T. 

1231, N. 

1237, N. 

1244, N. and H. T. 

1252, N. — Streaky. 

1285, N. 

1286, N. and H. T. 



The normalized, as v/ell as the heat-treated specimens, were 
partially decarburized uniformly to the depth of 0.005 iiich along 
the gage length of the tension specimen, which makes o. 010. inch 
of the diameter of the gage length decarburized. The dijEferences 
in the microstructures of the air-cooled specimens have already 
been described. In the heat-treated specimens those that gave 
the best results in the tension tests invariably had a structure of 
fine martensite. Wherever appreciable amounts of ferrite were 
found, together with the martensite in the quenched and tempered 
specimens, the tension values were not so good. In many cases 
unexpected low results could be traced to the presence of rela- 
tively large amounts of ferrite (see Fig. 13). The variations in 
the drawing temperatm"es, if there were any, could not be detected 
in the microstructure. 

Altogether, in this part of the examination 160 micrographs of 
the steels in the cast, rolled, and finally heat-treated conditions 
were taken. For lack of space they can not be given here, but 
they were invaluable in helping to interpret the results of the 
mechanical tests. By means of this survey of the microstructures 
of the samples those containing flaws were discovered and elimi- 
nated, and any irregular results could be explained. The micro- 
scopic "check-up" thus served to relieve any doubts concerning 
single samples,and helped to give weight to the general conclu- 
sions of the investigation. 



140 Technologic Papers of the Bureau of Standards [Voi.16 

3. MECHANICAL PROPERTIES 

(a) TENSILE TESTS 

Since the rolled material was one-half inch or less in thickness, 
it was impossible to use the standard form of tensile specimen 
having a diameter in the reduced section of 0.505 inch. A shoul- 
der type specimen was used, having a diameter of 0.300 inch at 
the reduced section and a gage length of 2 inches, as shown in 
Fig. 14. This ratio of gage length to area of specimen gives values 
of elongation somewhat less than would be obtained with standard 
size specimens, and this fact should be borne in mind in inter- 
preting the results. The tensile and also the impact specimens 




^as long as possible 

Fig. 14. — Dimensions of tensile specimens 

were completely machined before heat treatment and not ground 
before testing. 

Tensile tests were made on either a 50 000-pound or 100 000- 
pound Riehle testing machine. Proportional limit was deter- 
mined from plotted stress strain curves, strain being measured 
by means of a Berry strain gage. In a few cases the specimens 
were too short to admit of fastening a strain gage to the specimen, 
and blanks appear in the tables (Tables 11-22) for these cases. 
Yield point was determined by the " drop-of-the-beam " method 
where any " drop " was observed. Reduction of area and elonga- 
tion were obtained by the usual measurements after fracture. 

Tables 11-22 give the results of the tensile tests on all the 
steels. It will be noted here that several of the steels have a 
tensile strength of well above 300 000 lbs. /in. ^, accompanied by 
appreciable ductility. No. 1207, with a tensile strength of 
344 000 lbs. /in. ^ was the highest value observed.* 



Burgess l 
Woodwards 



Zirconium Steels 



141 



TABLE 5. — Hardness Measurements on Plate 

[ *Indicates specimen not completely broken] 





Thick- 
ness 


Hardness numerals 


Ingot No. 


Thick- 
ness 


Hardnessnumerals 


Ingot No. 


Brinell 


Sclero- 
scope 


Brinell 


Sclero- 
scope 


1101 


Inch 

Vs 
H 
% 
Vi 
% 

% 
J4 

Vi 
Vs 
'A 
% 
'A 
% 
A 

Va 
A 
H 
A 
Va 
A 
% 

H 
A 

Va 
A 

H 

Va 
A. 
Va 
A 

Va 
A 

Va 
A 
Va 
A 
Va 
A 
Va 
'A 

Va 
A 
Va 

'^ 

^a 

1 


334 293 
405 444 
240 245 
217 223 
207 207 
223 212 
207 194 
187 205 
172 241 
232 207 

189 235 
202 216 
189 182 
187 196 
236 231 
244 255 
317 335 
340 351 
415 302 
290 438 

467 244 
477 484 
537 491 
555 520 
364 354 
361 340 
626 508 
600 576 
626 626 


30 26 
52 47 

27 25 
21 22 

23 23 

32 31 
20 21 

20 22 

28 28 
30 28 

24 25 

21 26 

22 20 
20 21 
24 .. 
26 .. 
30 .. 

33 .. 
41 31 
39 40 

39 34 
43 43 
48 49 
62 60 

34 37 
47 42 
43 43 
57 68 
54 54 


1159 


Inch 

Va 
A 
Va 
A 
Va 
A 
% 
A 


294 327 
503 477 
573 279 
556 545 
285 440 
432 512 
321 337 
387 338 
219 234 

375 340 
338 346 
430 514 
364 387 
421 385 

640 571 
550 600 
387 447 
424 428 
328 302 

226 206 
472 467 

470 481 
477 477 
196 211 

208 216 
213 224 
257 241 
171 172 
211 244 

381 403 
300 311 
342 336 
351 360 
351 325 

344 338 
228 217 
252 233 
439 457 
444 403 

465 398 
415 369 

209 218 
216 210 
321 302 

268 266 
207 199 
477 457 
505 512 
481 491 

627 600 
629 616 
600 555 
378 411 
456 447 

367 361 

471 564 
481 495 
600 553 
418 387 

475 477 
310 278 
235 228 
441 337 
312 323 


32 32 


1102 


1160 


55 45 


1103 


1161 


60 52 
24 42 


1104. . 


116^2.. 


31 47 
24 23 


1105.. .. 


1163 


38 37 
21 22 




1164 




30 28 




1165* 












1166... 








1167 












1168... 




44 43 




1169 






1111. 






1170 




61 57 


1112. 


1171 




34 41 




1172 




43 37 




1173 




28 26 


1113 


1174 








19 19 


1114 


1175* 




52 52 




1176 




36 38 


U15. 


1177*. . 




55 55 




1180 




19 23 


1117 


1181 








20 21 




1182 




20 21 




1183.. 








387 364 
555 600 
495 470 
418 495 
380 370 
467 418 
444 387 
475 460 
387 370 
338 375 

652 635 
575 534 
558 552 
589 626 
387 488 
444 402 

477 470 
444 477 
444 336 
512 444 

491 479 
410 375 
589 608 
578 591 
578 346 
589 555 
351 245 
444 352 
418 390 

478 321 

487 450 
387 477 
585 555 
519 550 
477 516 
537 534 
418 423 
518 522 
544 640 
452 452 


42 40 

54 52 

52 43 
47 52 
35 36 
42 45 

39 42 
47 42 
37 35 
37 35 

"53"63 

■■55' '65 

40 54 
45 40 

42 48 

55 58 

'"47"43 

'"37' "34 

"'56"56 

53 26 

55 50 
35 25 

41 31 
32 32 
45 28 

52 60 

37 45 

""5i"S3 

43 45 

56 55 

38 39 
55 59 

""56"51 


1184 




18 19 


1119 


1185 






1120 


1186.. . 








1187 






1128 


1188 








1189* 




42 44 


1129 


1190 




34 29 


1130 


1191 




29 28 




1192 




24 23 




1193.. .J 


26 26 


1131. 


1194 1 


52 53 




1195 ..i -- 


42 38 




1196 








46 34 


1133. 


1197 




36 36 




1198 




23 24 


1134.. 


1199 --- 


24 23 




1200 




37 28 




1201 








26 26 




1202 




21 21 


1136 


1204* 




50 53 




1205 




41 45 


1138 


1206 




42 47 


1144 


1207 




55 55 




1208. 


- 


69 61 


1145 


1209 




66 62 




1210 




38 44 


1146. 


1211 




46 40 




1212* 




43 45 


1147. 


1213 




42 51 




1214 




41 37 




1215 




53 48 




1216 




34 35 


1156 


1217 








55 55 


1157. 


1218 ! 


30 28 




1219 . ' 


23 23 




1220 


45 36 




1221 


33 33 



142 Technologic Papers of the Bureau of Standards ivoi. ts 

TABLE 5. — Hardness Measurements on Plate — Continued 
[ *Indicates specimen not completely broken] 





Thick- 
ness 


Hardness numerals 


Ingot No. 


Thick- 
ness 


Hardness numerals 


Ingot No. 


Brinell 


Sclaro- 
scope 


Brinell 


Sclero. 
scope 


1222* 


Inch 


366 367 
357 317 
406 438 
467 387 
430 454 

550 537 
629 627 
585 573 
603 605 
520 474 

494 505 
321 311 
364 375 
351 241 
484 472 

600 585 
444 474 
532 555 
509 515 
520 512 

387 430 
460 438 
441 420 
525 493 
444 444 

366 418 
248 256 
361 371 
324 324 
477 495 

477 487 
600 560 
532 495 
524 477 
441 440 


47 49 
33 26 
32 34 

32 41 
36 37 

54 54 
66 62 
57 55 
70 69 
47 42 

44 46 
28 26 
30 30 
23 22 
54 53 

56 54 

46 49 
59 61 

41 42 

47 47 

39 41 

42 43 
44 45 
56 57 
39 35 

33 36 
20 20 
19 18 
28 26 

39 37 

40 39 
53 49 
49 49 
52 47 
38 40 


1259.. 


Inch 


596 605 
532 569 
207 223 
402 373 
387 396 

180 183 
252 219 
207 188 
351 364 
341 342 

250 321 
255 216 
444 418 
555 600 
534 570 

410 444 
395 397 
490 520 

510 486 
508 468 

510 475 

539 512 
475 430 
520 508 

340 447 
455 498 
464 478 
522 486 
418 470 


47 48 


1223 




1260... . 


57 48 


1224 




1261 : . . 


18 19 


1225. 




1263. 


37 40 


1226 




1264 


43 43 


1227. 




1 

1267*. ' 


27 25 


1228 ' 


1268 


23 22 


1229 1 


1269* 




1230. 1 


1270*. 


20 21 


1231 


1271* 


38 40 


1232. ' 


1272*.. 




25 30 


1233 .1 


1273* 




32 24 


1234 


1274* 




52 43 


1235 


1275* . 




55 60 


1236 


1276* 




52 54 


i 
1237 ' 


1277* 




42 51 


1238... 1 - -- 


1278* 




44 43 


1239 




1279* 




50 60 


1240 




1280* 




60 57 


1241... 




1281* 




60 59 


1242 




1282* 




57 53 


1243.. 




1283* 




57 58 


1244 




1285* 




49 47 


12«* 




1286* 




54 52 


1246 




1289* 










38 49 


1247 


1290* 




51 55 


1243. 




1291*.. 




50 49 


1249. . 




1292* 




60 60 


1250 




1293* 




39 47 


1251 










1252. 






1253 






1256 






1257. 






1258 













(b) IMPACT TESTS 

Impact tests were made on heat-treated specimens from all 
heats beyond No. 1155 and a few previous, the heat treatment 
being the same as for the tensile specimens and plates. Hardness 
tests made on a few impact specimens gave sufficient evidence 
that the impact specimens were in a structural condition similar 
to the tensile specimens. An Izod machine using a cantilever 
type of specimen was used in all impact tests. 

Here, again, the thickness of the available material precluded 
the use of the standard type of specimen in all cases. For those 
plates which would not admit of making a roimd specimen 0.450- 
inch diameter (see Fig. 15), the largest diameter possible in multiples 
of 0.050 inch, v/as used and the notch made geometrically similar 
to the larger specimens. The total length of the specimens re- 



wfJdward] Zirconium Steels 143 

mained constant, so as not to alter the striking distance. The 
specimens of small size were held in the anvil of the impact ma- 
chine by means of hardened steel split sleeves having an outside 
diameter of 0.450 inch and an inside diameter to fit the specimen. 
This sleeve was inserted in the anvil flush with its top surface and 
the impact specimens properly aligned by means of a templet. 
The height of fall of the pendulum was varied proportionally to 
the size of the specimen, although theoretically this should not be 
necessary. 

The area of the specimens at the notch was computed and the 
energy absorbed in breaking for unit area determined, a value 
which has been called the specific impact work. The results of 
the tests are given in Table 6. While the law of similarity has not 
been definitely shown to hold for impact specimens as for other 





Fig. 15. — DiTnensions of impact specimens 

forms of mechanical testing, the method used was considered the 
most desirable that the circumstances would permit. 

A high impact value does not always indicate a superior steel, 
since such values are many times accompanied by low tensile 
strength. Thus, all the steels which had an impact value greater 
than 200 foot-pounds per square inch also gave tensile strengths 
less than about 130000 Ibs./in.^ except No. 1252, which had a 
tensile strength of 324 800 lbs. /in. ^ On the other hand, if we 
select all those steels which showed an impact value less than 50 
we note that the majority of that group have a tensile strength 
in excess of 275 000 lbs. /in. ^, although a few fall even below 
100 000 lbs. /in. ^ the latter being clearly inferior steels. Those 
steels, then, that show fair values of impact, together with high 
tensile strength, should be considered the best steels, since they 
combine strength with toughness. 



1 44 Technologic Papers of the Bureau of Standards 

TABLE 6.— Impact Tests (Izod Machine) 
[^Indicates specimen not completely broken] 



[Vol. i6 



Ingot No. 



Diame- 
ter ol 
specimen 



1135.. 
1136.. 
1138.. 
1155.. 
1156.. 

1157.. 
1158.. 
1162.. 
1163.. 
1164.. 

1165.. 
1166.. 
1167.. 
1168.. 
1169.. 

1170.. 
1171.. 
1172. 
1173.. 
1174.. 

1175.. 
1176.. 
1177. 
1178. 
1180. 

1181.. 
1182.. 
1183.. 
1184.. 
1185.. 

1186.. 
1187. 
1188. 
1189. 
1190. 

1191. 
1192. 
1193. 
1194. 
1195. 

1196. 
1197. 
1198. 
1199. 
1200. 

1201. 
1202. 
1204. 
1205. 
1206. 

1207. 
1208. 
1209. 
1210. 
1211. 

1212. 
1213. 
1214. 
1215. 
1216. 

1217. 
1218. 
1219. 
1220. 
1221. 



Inch 

0.450 
.450 
.447 
.447 
.447 

.450 
.448 
.445 
.448 
.347 

.449 
.346 
.350 
.450 
.347 

.351 
.454 
.354 
.353 
.449 

.447 
.354 

'"""."456' 
.450 

.296 
.445 
.349 
.444 
.446 

.441 
.349 
.348 
.350 
.450 

.354 
.450 
.354 
.447 
.349 

" .347 
.348 
.449 
.345 
.447 

.349 
.452 
.449 
.350 
.349 

.350 
.446 
.350 
.446 
.348 

.447 
.447 
.349 
.447 
.448 

.350 
.349 
.448 
.447 
.353 



Area at 
notch 



Inch' 

0. 1210 
.1210 
.1196 
.1196 
.1196 

.1210 
.1201 
.1187 
.1201 
.0732 

.1206 
.0730 
.0736 
.1210 
.0732 

.0738 
.1229 
.0742 
.0741 
.1206 

.1196 
.0742 

'"'ino 

.1210 

.0524 
.1187 
.0735 
.1182 
.1192 

.1168 
.0735 
.0733 
.0736 
.1210 

.0742 
.1210 
.0742 
.1196 
.0735 

.0732 
.0733 
. 1206 
.0729 
.1196 

.0735 
.1220 
.1206 
.0736 
.0735 

.0736 
.1192 
.0736 
.1192 
.0733 

.1196 
.1196 
.0735 
.1196 
.1201 

.0736 
.0735 
.1201 
.1196 
.0741 



Initial 
energy 



Ft.-lbs. 
120 
120 
120 
120 
120 

120 

120 

120 

120 

75 

120 
75 
75 

120 
75 

75 

120 

75 

75 

120 

120 
75 

m 

120 

60 
120 

75 
120 
120 

120 
75 
75 
75 

120 

75 
120 

75 
120 

75 

75 
75 

120 
75 

120 

75 

120 

120 

75 

75 

75 
120 

75 
120 

75 

120 
120 
75 
120 
120 

75 

75 

120 

120 

75 



Energy absorbed 
In breaking 



Ft.-lbs. 

7.0 
8.0 
6.5 
13.5 
5.0 

13.5 
5.5 
6.0 

29.5 
8.0 

9.5 
8.0 
4.5 



4.5 
16.5 
11.0 

9.0 
16.0 

10.5 
8.0 

"9.' 5 

14.0 

6.5 
15.0 

6.0 
28.0 
42.0 

19.0 
9.0 

10.0 
8.0 

14.5 

7.5 
24.5 
17.5 
10.5 

7.5 

9.S 

8.5 

75.5 

33.5 

14.5 

16.0 

41.5 

12.0 

7.0 

9.5 

5.5 
4.5 
1.5 
14.0 
9.5 

12.0 
4.5 
6.5 
6.0 

13.5 

6.5 
9.0 
17.5 
9.0 
9.0 



Ft.- 
Ibs./in.' 
58 
66 
54 
113 
42 

112 
46 
51 

246 

109 

79 
110 
61 
99 
75 

61 
134 
148 
121 
133 



108 

'"78 
116 

124 
126 
82 
237 
357 

163 
122 
136 
109 
120 

101 
202 
236 
88 
102 

130 
116 

*625 

*460 

121 

218 
340 
100 
95 
129 

75 

38 

20 

117 

130 

100 
38 
88 

50 
112 



122 

146 

75 

121 



Burgess T 
Woodwardj 



Zirconium Steels 



145 



TABLE 6.— Impact Tests (Izod Machine)— Continued 
[^Indicates specimen not completely broken] 



Ingot No. 


Diame- 
ter of 
specimen 


Area at 
notch 


Initial 
energy 


Energy absorbed 
in breaking 


1222 


Inch 
0.450 
.449 
.353 
.349 
.298 

.299 
.299 
.348 
.296 
.350 

.299 
.300 
.349 
.350 
.349 

.351 
.298 
.299 
.299 
.298 

.351 
.300 
.349 
.299 
.300 

.350 
.351 
.349 
.299 
.299 

.298 
.298 
.450 
.400 
.350 

.399 

.400 
.449 
.400 
.450 

.398 
.400 
.449 
.398 
.449 

.397 
.397 
.389 
.450 
.450 

.348 
.450 
.448 
.448 
.449 

.450 
.449 
.449 
.449 
.349 

.350 
.349 
.350 
.349 


Inch' 
0.1210 
.1206 
.0741 
.0735 
.0534 

.0539 
.0539 
.0733 
.0524 
.0736 

.0539 
.0544 
.0735 
.0736 
.0735 

.0738 
.0534 
.0539 
.0539 
.0534 

.0738 
.0544 
.0735 
.0539 
.0544 

.0736 
.0738 
.0735 
.0539 
.0539 

.0534 
.0534 
.1210 
.0833 
.0736 

.0827 
.0833 
.1206 
.0833 
.1210 

.0821 
.0833 
.1206 
.0821 
.1206 

.0815 
.0815 
.0827 
.1210 
.1210 

.0733 
.1210 
.1201 
. 1201 
.1206 

.1210 
.1206 
.1206 
.1206 
.0735 

.0736 
.0735 
.0736 
.0735 


Ft.-lbs. 

120 

120 

75 

75 

60 

60 
60 
75 
60 
75 

60 
60 
75 
75 
75 

75 
60 
60 
60 
60 

75 
60 
75 
60 
60 

75 
75 
75 
60 
60 

60 

60 

120 

100 

75 

100 
100 
120 
100 
120 

100 
100 
120 
100 
120 

100 
100 
100 
120 
120 

75 
120 
120 
120 
120 

120 
120 
120 
120 
75 

75 
75 
75 
75 


Ft.-lbs. 
11.0 
9.5 
7.5 
8.5 
4.5 

4.0 
2.0 
8.0 
.5 
8.0 

4.0 
4.0 
6.5 
13. S 
8.5 

4.5 
4.5 
1.0 
6.5 
1.5 

6.5 
7.5 
7.5 
3.5 
2.5 

4.0 
6.0 
10.0 
5.5 
2.0 

13.5 
2.5 

21.5 
6.0 
5.0 

8.0 
6.0 
5.8 
4.0 
5.5 

3.0 
6.0 
14.5 
10. S 
10.5 

10.5 

31.0 

3.0 

5.0 

4.2 

8.0 
19.5 
4.0 
6.0 
4.0 

7.0 
3.0 
10.0 
8.0 
7.0 

6.0 
5.5 
5.5 
7.0 


Ft.- 

lbs./in,» 
91 


1223 


79 


1224 


101 


1225 


116 


1226 


83 


1227 


74 


1228 


37 


1229 


109 


1230 


10 


1231 


109 


1232 


74 


1233 


74 


1234 


88 


1235 


183 


1236 


116 


1237 


61 


1238 


84 


1239 


19 


1240 


120 


1241 


28 


1242 


88 


1243 


138 


1244 


102 


1245 


65 




46 




54 


1248 


81 




136 


1250 


102 




37 




252 


1253 


47 


1256 


174 


1257 


72 




68 




97 


1260 


72 




48 


1263 


48 




46 




37 


1268 


72 


1269 


120 


1270 


128 




91 




128 


1273 


380 




36 


1275 ; 


41 




35 




103 


1278 


161 


1279 


34 


1280 


50 




33 




58 


1283 


25 




83 


1286 


66 




95 




82 


1291 


75 


1292 


75 


1293 


95 







146 



Technologic Papers of the Bureau of Standards [Voi.16 



(c) HARDKESS TESTS 



Hardness tests were made on the tensile specimens and on the 
hardened plates. For the tensile specimens this consisted of two 
Brinell impressions on the ends of the broken specimens after 
grinding off the outside smiace. Scleroscope hardness was also 
determined on the same material, several readings being taken 
with a recording scleroscope. 

On the plates opposite comers were gromid down and duplicate 
Brinell and several scleroscope determinations made at each posi- 



Kica 
















' 
















^ 


-p, 


H 


— 


' 


■ 









' ^■ 






' 










-•" 


^ 




- 





























































5RINEUI. HARDNE55 NUMERAL 



Fig. 16. — Relation between tensile strength and Brinell hardness 

lion. In this case an indicating scleroscope was used for some of 
the work and a recording instrument for the remainder. The 
indicating instrument gave uniformly lower values than the re- 
cording t5rpe, so that the scleroscope values for the plates are not 
in all cases intercomparable. Those taken with the latter instru- 
ment are marked with an asterisk in Table 5, which gives the hard- 
ness values for both comers of each plate. 

The method of heat treatment described in Section III-2 does 
not give exactly the same hardness to both the small tensile speci- 
mens and the relatively larger plates. To secure the same hard- 
ness, it would have been necessary to draw back the tensile speci- 
mens at varying temperatures until like conditions were reached. 



wZwarA Zirconium Steels i^j 

B}^ aid of Fig. i6, showing the relation between tensile strength and 
hardness for this class of steels, an idea of the actual tensile prop- 
erties of the hardened plates may be obtained. 

V. COMPARISON TESTS ON SIMILAR MATERIAL 

In addition to the ingots prepared by the Bvireau of Mines there 
was also available for study other material of a similar nature 
which was submitted through the Bureau of Ordnance of the Navy 
Department and was secured from one of the large automobile 
manufacturers who was constructing armored tanks during the 
war and whose representatives had made great claims for zirconium 
as an alloying element in light armor plate. This material con- 
sisted of 45 plates of X "to H inch thickness, representing 28 sepa- 
rate heats of steel. Each heat, comprising about 1000 pounds of 
metal, was made in an electric furnace. 

The majority of the plates as submitted were 18 inches square. 
The following, however, were 12 inches square: 16-1, 19-1, 20-3, 
22-2, 22-3, 22-4, 24-5, 25-1, 25-2, 25-4, 25-8, 27-3, and 27-4. 
(The first number in all cases refer to the heat number and the 
second to the plate number of that heat.) The plates were sup- 
posedl}^ heat treated, but many were found to be soft and were 
heat treated at the Bureau of Standards in accordance with a 
summary of the heat treatments given the same material by the 
manufacturer. 

All plates were cut up, the hardened ones by grinding, so as to 
produce two tensile bars, an impact specimen, and a 12 by 12 inch 
ballistic plate from the large size plates. From the smaller 
plates a ballistic plate of 1 1 by 1 1 inches was obtained in most cases. 

In Table 7 is given the heat treatment of the plates and test 
pieces on those plates which were heat treated at the Bureau of 
Standards. 

The same type of specimen and testing procedure was used for 
these materials as for those described above, with the exception 
that the B and C specimens are both hardened and no tests were 
made on normalized material. 

In Table 12 will be found the results of impact tests calculated 
in a similar manner to those given before. 

A comparison of these tests made at the Bureau and t^hose 
made by the manufacturer is given in Table 9, the average value 
for each heat being given. In the grand average certain of the 
heats are omitted, as noted in the table, since the figiures from 
both sources are not strictly comparable. 



148 Technologic Papers of the Bureau of Standards [Voi.td 

TABLE 7, — Comparison Steels 



[AC= 


Air cooled 


; FC=fumace cooled. All specimens drawn Jor one 


hour in oil bath unless otherwise 








stated] 








Temperatures 








Temperature 


s 




Heat 
No. 






Remarks 




Heat 
No. 










Normal- 


Quench- 


Draw- 


Normal- 


Quench- 


Draw- 


Remarks 




izing 


mg 


mg 








izmg 


mg 


ing 






"C 


°C 


°C 








°C 


•c 


°c 




2.... 


870 AC 


850 


205 






18.... 


870 FC 


850 


190 




4 


870 AC 


850 


205 






19 


816 AC 


860 


190 




6 


870 FC 


850 


205 






20 


954 AC 


850 


316 


Salt bath lor 


8.... 


870 FC 


850 


193 














drawing 


9 


870 AC 


830 


193 






21.... 
22 


870 FC 
870 FC 


850 
850 


190 
190 


Drawn for three 


10.... 


870 AC 


830 


193 














hours 


11 


870 FC 


777 


177 






23 


870 FC 


827 


205 




12 


870 AC 


843 


205 






24 


870 AC 


860 


205 




13 


870 FC 


850 


205 
















14 


870 FC 


843 


288 


Salt bath 
drawing. 


for 


25 

26 

27.... 


900 FC 
800 AC 
816 AC 


850 
800 
843 


205 
200 
204 




15 


870 FC 


827 


290 


Do. 




280... 


800 AC 


800 


200 




16.... 


870 FC 


830 


193 

















" These values not given by manufacturer, but estimated at Bureau of Standards. 

Table 10 gives the results of hardness measurements on ground 
portions of opposite comers of the plates. The results that were 
obtained on these comparison steels are quite similar to those 
obtained on otu* own material, but it will be noted that the highest 
tensile properties observed were not so great as those from the 
regular series. The comparison steels will therefore be included 
in the discussion of results and the effect of the various elements 
on the properties of steel. 

TABLE 8. — Impact Tests (Izod Machine) of Comparison Steels 



steel 


Diameter 
of spec. 


Area at 
notch 


IniUal 
energy 


Energy absorbed 
in breaking 


2-1 


Inch 

0.449 
.397 
.448 
.399 
.449 

.400 
.450 
.400 
.399 
.499 

.399 

.400 
.349 
.450 
.349 

.348 
.449 
.349 
.450 
.449 

.449 
.349 
.348 
.398 
.449 

.398 
.349 
.301 
.349 
.450 


Inch: 

0. 1206 
.0815 
.1201 
.0827 
.1206 

.0833 
.1210 
.0833 
.0827 
.1206 

.0827 
.0833 
.0735 
.1210 
.0735 

.0733 
.1206 
.0735 
.1210 
.1206 

.1206 
.0735 
.0733 
.0821 
.1206 

.0821 
.0735 
.0549 
.0735 
.1210 


Ft.-lbs. 
120 
100 
120 
100 
120 

100 
120 
100 
100 
120 

100 
100 

75 
120 

75 

75 
120 

75 
120 
120 

120 

75 

75 

100 

120 

100 
75 
60 
75 

120 


Ft-lbs. 

17.0 
6.0 
4.0 

12.0 
4.0 

3.5 
14.0 
14.0 
13.0 

6.0 

15.0 
6.0 
3.0 

15.0 
7.0 

5.5 
6.0 
8.0 
16.5 
9.0 

9.0 
9.0 
7.0 
11.0 
9.0 

10.5 
2.0 
4.0 
R. 

4.0 


Ft.- 
Ibs./in.2 
141 


4-1 


74 


6-1 


34 


8-1 


145 


9-1 


33 


9-2 


42 


10-2 


116 


11-2 


168 


12-1 : 


157 


13-2 


50 


14-1 


181 


15-1 


72 


16-1 


41 


18-1 


124 


19-1 


95 


20-1 


75 


20-3 ... 


50 


22-1 


109 


22-2 


136 


22-3 


75 


22-4 


75 


23-1 


123 


24-5.... 


96 


25-1 


134 


25-2 


75 


25-4 


128 


26-1 


27 


27-3 


73 


27-4 


109 


28-1 


33 







Burgess "1 

Woodivardi 



Zirconium Steels 



149 



1 


3 

s 




s 


§ 


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t-l 




«> 


T) 


A 




a 


•c 


s 


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w 


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& 

O 

U 



CO 



01 V l-i 









M a 
eu a 

5" 



1=1 



CO" 



d 

3 <a 
PS" 



as 

S.S 









m t> r^ (M in 

m o- "o CO ij-i _ _ 



ou-jcjvotM Tf 10 00 »n 00 (Nit^comTj- rj fsj ■^ (M -^ 

o to i-< ^o CO ■* irj t*^ -^ c^ .-H t^ -^ m CO r-i i-t co ro ■<)- 

Tj-iomioio lo-o-invnn io>o»/j>n>n 



^ owi 00 CO ■<J- 
5? uS t-J CO CO «> 



.^ m in 00 o o 



A< 



X m o o m o o o o 



m tn o o 

vo >A i-i O 



inio o CO o 
CO TT 00 ■-< 



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m c>.o CO 
00 oco c5 



m oco imn 



„ 00000 
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C o o tn o o 

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M inco «o o vo 

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rfS ■* o ' o 

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CO 00 -(d- 00 00 
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CM CM *-< CO eg 



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150 Technologic Papers of the Bureau of Standards 

TABLE 10.— Comparison Steels 
[Hardness of plates on opposite comers] 



[Vol. 16 





Hardness numeral 


Plate No. 


Hardness numeral 


Plate No. 


BrineU 


Sciero- 
scope 


BrineU 


Sclero- 
scope 


1-3 


532 495 
418 402 
375 387 
607 532 
510 495 

311 311 
600 546 
600 600 
555 578 
477 495 

600 555 
512 495 
474 452 
560 555 
555 568 

508 512 
418 418 

509 512 
258 262 
567 522 

504 500 
512 486 
477 460 


61 06O 

49 47 
44 045 

62 "61 
53 51 

38 "38 

57 «55 

65 65 

63 67 

55 "57 

58 055 
62 06O 
53 52 

66 65 
61 63 

57 63 

56 53 

65 67 
33 035 

66 64 

66 59 
60 59 

50 49 


17-1 


262 262 
512 526 

273 277 
486 522 
293 293 
504 516 
514 571 

474 470 
514 479 
553 512 
495 474 
474 465 

571 544 
532 483 
522 518 
529 553 
510 526 

544 550 
562 562 
407 446 
439 452 
522 480 


29 


2-1 


18-1 


60 30 


2-2 


18-2 


62 


3-1 


32 a 


4-1 


19-1 


58 5 




19-2 


32 a 33 


4-2 


20-1 


56 57 


5-1 


20-3 


57 66 


5-2 


21-1 




6-1 


58 56 


6-2 


22-1 


61 58 




22-2 


67 55 


7-1 


22-3 


58 47 


7-2 


22-4 


47 44 


8-1 


23-1 




9-1 


72 68 


9-2 


24-5 


64 58 




25-1 


56 55 


10-2 


25-2 


59 61 


11-2 . 


25-4 


57 61 


12-1 


25-8 




13-1 


65 67 


13-2 


26-1 


71 69 




27-3 


47 48 


14-1 


27-4 


53 54 


15-1 


28-1 


60 54 


16-1 













" Plates not heat treated at Bureau. 

VI. EFFECT OF VARIOUS ADDITION ELEMENTS 

The large number of steels examined offers an excellent opportu- 
nity for studying the effects of the various alloying elements. In 
nearly all the heats, however, the silicon content is higher than that 
usually obtained in ordinary practice . For purposes of comparison 
it is necessary to classify the steels into groups having the least 
possible number of variables in each group. The carbon content 
is a variable in practically every group, and the arrangement given 
in the tables is according to increasing carbon content. 

The groups into which the steels have been roughly classified 
are as follows: Group A, silicon steels; Group B, nickel-silicon 
steels; Group C, silicon-zirconium steels; Group D, nickel-sili- 
con-zirconium steels; Group B, cerium steels; Group F, copper 
steels; Group G, boron steels ; Group H,xu-anium steels; Group I, 
molybdenum steels; Group J, nickel-chromium steels; Group K, 
vanadium steels; Group I/, chromium- tungsten steels; Group M, 
cobalt steels. 



Woodward] Zircouium Stcels 151 

1. GROUP A— SILICON STEELS 

This group, shown in Table 1 1 , represents plain carbon steels 
in which the silicon is greater than normal and which have all been 
deoxidized with aluminum. The group has been further divided 
into steels that have greater or less than i per cent silicon. It 
will be noted that the increase of silicon to above i per cent has 
resulted in a greater tensile strength and impact value without 
materially reducing the ductility. Nos. 1269 and 1 2 70, containing, 
respectively, 0.65 per cent titanium and 0.45 per cent aluminum, 
show no superiority over No. 1104, which is simply deoxidized 
with these elements. 

2. GROUP B— NICKEL-SILICON STEELS 

Table 1 2 illustrates this group which has been further classified 
into steels containing 2 per cent nickel, 3 to 3.25 per cent nickel 
with silicon greater or less than i per cent, and those having more 
than 3.25 per cent nickel. 

The class with 2 per cent nickel all contain approximately i 
per cent silicon and show increased mechanical properties in com- 
parison with the corresponding class of Group A. A few steels 
in this class have tensile strength in the neighborhood of 300 000 
lbs. /in. ^, but the ductility and toughness are not as great as in 
those that follow. 

The 3 per cent nickel group again shows the advantage of in- 
creasing the silicon to greater than i per cent. In fact, this combi- 
nation of elements represents about the best of any of those tested, 
the majority having a tensile strength from 270000 to 315 000 
lbs. /in. ^, depending upon the carbon content, yield point from 
200000 to 250000 Ibs./in.^, and proportional limit from 100 000 
to 160000 lbs. /in. ^, excellent ductility and satisfactory impact 
values. The values for the normalized steels are also excellent. 
A cai:bon content of from 0.40 to 0.50 seems to be the most 
favorable. 

The nickel content apparently should be kept in the range 3 to 
3.25 per cent, as those steels having a higher percentage than this 
were nearly all brittle. 

Group B also shows, as did Group A, that aluminum and tita- 
nium in amounts greater than that needed for deoxidation offer 
no advantage and, in fact, appear to be in most cases detrimental. 



152 Technologic Papers of the Bureau of Standards [Voi. 16 

3. GROUP C— SILICON-ZIRCONIUM STEELS 

This group as tabulated in Table 13 should be compared with 
Group A, which contains similar steels without zirconium. The zir- 
conium content is variable from a small amoimt to 0.60 per cent. 
A study of Tables 11 and 13 seems to indicate that in the steels 
of lower carbon content the zirconium may have increased the duc- 
tility but not the tensile strength for the heat-treated steels. In 
the higher carbon range the ductility is much less than for similar 
steels in which zirconium is absent. The normalized steels con- 
taining zirconium have lower proportional limit, yield point, ten- 
sile strength, and ductility than those of Group A. 

4. GROUP D— NICKEL-SILICON-ZIRCONIUM STEELS 

These steels shown in Table 14 are subclassified similar to those 
of Group B. The 2 per cent nickel steels do not give as great ten- 
sile strength with zirconium as without it, but seem to show greater 
ductility and toughness. The same may be said of the 3 per cent 
nickel steels, although in this case the ductility is not increased 
to as great an extent, if any. There are several places in the 
table where the carbon content is constant and zirconium prac- 
tically the only variable. None of these instances, however, show 
any regular effect on the properties attributable to the zirconium 

content. 

5. GROUP E— CERIUM STEELS 

The cerium steels without nickel, as shown in Table 15 and 
compared with the first portion of Group H, indicate that with 
about 0.25 per cent of cerium the tensile properties are increased 
with accompanying loss of ductility. The nickel-cerium steels 
have been arranged partly in order of cerium content in the table, 
since they are all of approximately the same carbon content. 
Although nearly all of the nickel-cerium steels have the nickel- 
silicon ratio shown in Group B to be desirable, it also appears 
that small amounts (up to o.io per cent) of cerium are beneficial, 
while larger quantities offer no fiurther advantage. No. 1260, 
with only o.oi per cent cerium, is a most excellent steel. 

The role of cerium is thought to be that of a desulphtuizer, and 
in Nos. 1256 and 1257 the sulphiw content was intentionally in- 
creased to investigate this point. The tensile strength of these 
two steels is quite high, but the ductility is less than would be 
expected from a consideration of the other constituents. In 
amounts over 0.30 per cent cerium segregates very badly, and 
accordingly it would appear preferable to keep it below this figure. 



teiord] Zirconium Steels 153 

6. GROUP F— COPPER STEELS 

The copper has been added to these steels in place of a portion 
of the nickel content, and an inspection of Table 16 indicates that 
in thos? steels in which the sum of the nickel and copper, together 
with the silicon and carbon, are in the favorable ratio the usual 
high tensile strengths are secured, but with a reduction of the 
ductility and toughness. Specimens Nos. 1279 and 1280, for 
instance, broke in the shoulders, while the impact values are 
mostly low. No. 1285, with 0.70 percent zirconium, apparently 
corrected for some of the lost ductility. 

7. GROUP G— BORON STEELS 

This group can almost be dismissed from further consideration 
because of manufacturing difficulties in producing sound steel 
containing boron. The majority of the steels (see Table 17) 
were of low carbon content, but do not compare favorably with 
similar steels of Groups H and B. The ductility is in all cases 
low even with small amounts (0.02 per cent) of boron. No. 1276, 
containing the favorable ratio of carbon, silicon, and nickel, did 
not show the high properties for that class. 

8. GROUP H— URANIUM STEELS 

There were only three steels containing uranium — Nos. 1228, 
1229, and 1244 — all having the favorable ratio of carbon, silicon, 
and nickel except No. 1228, which carried 0.63 per cent carbon. 
No 1 244 showed the usual high properties, but the other two were 
less desirable (see Table 22). 

9. GROUP I— MOLYBDENUM STEELS 

With the possible exception of Nos. 3, the molybdenum steels 
(see Table 18) do not show the remarkable ductility claimed 
elsewhere for this element.^ 

This may, of course, be due to type of heat treatment to which 
all of these steels were subject, but it is probable that all of the 
steels in the nickel-molybdenum series would have been superior 
for the purpose desired with the molybdenum omitted. 

5 Molybdenum as an alloying element in structural steels, G. W. Sargent, Proc. Am. Soc. for Test. Mats. 
20, Part n, p. s; 1920. 

63593°— 22 3 



154 Technologic Papers of the Bureau of Standards [Voi.td 

10. GROUP J— NICKEL-CHROMIUM STEELS 

The nickel-chromium steels classified in Table 19 all show 
good properties particularly regarding ductility and toughness. 
Although most of the steels contain zirconium also, the previous 
considerations would not indicate that this element has greatly 
influenced the results. The properties of all of the steels in 
Group J could be reproduced without the addition of either 
chromium or zirconium. 

11. GROUP K— VANADIUM STEELS 

This group contains the steel (No. 1207) which showed the 
highest tensile strength observed in the entire investigation — 
about 344 000 lbs. /in. \ Although the ductiHty is not so great 
as in certain of the other steels having very high tensile strength, 
it is nevertheless considerable for such a steel. In passing it 
might be worthy of mention that from a portion of the plate 
from this heat was constructed a spring for a precision aeronautic 
altimeter. This spring is constantly operating under a com- 
puted maximum fiber stress of 100 000 lbs. /in. ^ and shows no 
elastic hysteresis or aftereffect, which is common to springs in 
such instruments. The group, as a whole, shows good properties 
but can not be considered as preferable to Group B (see Table 20) . 

12. GROUP L— CHROMIUM-TUNGSTEN STEELS 

This group, consisting only of Nos. 11 77 and 11 78, comprises 
too small a number to permit drawing any conclusions, but appar- 
ently offers no particular advantages (see Table 22). 

13. GROUP M— COBALT STEELS 

The steels in this group (Table 21) are all from the comparison 
series. All except No. 15, which contained molybdenum in 
addition, showed high tensile strength, with good ductility and 
toughness. It is probable that cobalt acts similarly to copper 
in replacing some of the nickel. 



Btwgess "l 
Woodward} 



Zirconium Steels 



155 



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156 



Technologic Papers of the Bureau of Standards [Voi.i6 



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Burgess T 
Woodwards 



Zirconium Steels 



157 



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sis: 


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s s 2 g 

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d * ' * 


:: 13 s 3 



158 



Technologic Papers of the Bureau of Standards [Voi. i6 



I 
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S9 









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a 


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mrnotj^ o inooiooo-*-in o mooomotnenorHCMinoomTj-o 

OtOOO rH rHVD^OO^T-tO O OCM>-«rHr-(rgrHCTlOOOO^egrHOlI>eM 

rgcoeoeo eo eocMcocoeoeneocn en eocoeoeocncoeocMCOcncncMeocoeMeMeo 

■■ ■ ■ ' iJ 

«Otn»n to cnegoor^tOrHtMin oo ^oeo■«*•moorHOOfloeno■*■»:^tocnoJi 

^voioto at ctoocotnco<oooto cn inoooot>«oic7toococ»oooc^ooootooirH'0 

**'* * * ••••...••^ th3 

■ O 

inooo o ocMinooor-to o mmiftomootnintoinminoomo,ES 

<*-ininin i^ cocncnrHooo^ rH r-trHcocMOrHCMtoomtnaoocMrHOO cn 

^U^^ ^ ^^^^Cgr^rHi-; rH ^^^^WrH^r^r^rHrHr^rHrHr^r^rnO 

. ^ 

oocMCMCM CM '^^■*•t^"*mtototo to t>.t«.ooaiotoirHrHeneoenen^«n\o»oc^Ji4 

C4 eoeoff> eo cOeoencocnencoco eo eococoeocnco^^^^^^^'^^^^ O 

• Ih 

. . . . : ^^ — ^-^~. — r~T—. : r~. — : — r . . . . — r-~, — W 

(3 

lot^mto •-« Hf 'OtoOrH •■»»• 00 inco'^t^rHCMin -o •ot-^tooocM 't^ 

coatOtai rH eo >»-H»-ioteM • a\ rH egot-^meoeo'^ -cm 'Coco^eorH -rH 

(MrHrHrH N ^< "etaeMCMCMrHrH CM CM-CMrHrHrHrHi-H •CM^eMCMrHrHrHinrH 



l62 



Technologic Papers of the Bureau of Standards [Voi. i6 



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g 


00 
00 


g~ 


g 


s 







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c^ 




o» 


■<- CO CO 


to 


»-l 





CO 




S " 


-e- 




CO 


CO to t^ 


00 


at 




■^ 




— i- 


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00 




•* 


■* t-- CM 


m 





t^ 


in 




p« 


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^4 1-4 •-« 






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' 

















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. 

















01,9 


51 « 


CM 




CO 


■ CM 


\o 





CO 








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B u> 


,_( 




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CM 


-IT 


w 








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• 00 


■* 


t^ 












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to m m 




m 





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m 


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m 


in 10 


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« 


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CO 







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CO 


CO to 


CM 


to 







ft-° 






d 




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n 


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H 


iii 




; 






m 


c 


m 





m 


m 







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ts 








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to 


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a 


























^ : 








CM 


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c3 


CO 


CM 


CM 


CM 






















1 


1 


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0\ 






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m 







CM 


s 




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d 


c^ 01 


iH 


o\ 


a\ 


OC 





























■« w^ 


t^ 







xTi 








m 


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m 






« c^ 


CM 




CO 


c^ xn 


00 


CO 


CM 


w 


CO 




CO 


























dJ 






rH 


f-l fH 




•^ 




1-^ 


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»n 


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CM 


^ 


o\ 


^ 


f>4 







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■* 




■* 


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■* 


<r 


CO 


t^ 


in 




A 






d 



















































e 


^ 


































CC 


<M 1 






10 I> 


at 


CM 


<x 


cr 


— • 1 






vC 


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m un 


m 


tn 


in 


tn 


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CM 


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CM 1 








t-t 








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*-< 


f-< 


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164 



Technologic Papers of the Bureau of Standards Woi. 16 



4> 



M 






o 

6 



< 











e* 


m 




















s 


•..<3 


CO 


to 


«o 


UO 










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a 

1-4 




















2g. 

<u S 















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m 






m 


m 


<£l 


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VO 


m !>• 




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s 


l^ 


















a 
■g 


a 


































<S 


3 


I ^^ 




<M 


\o 


iri 





m 


CM 




« 




&i 






M- 


\n 


10 


p^ 


CO -^ 








•* 


Ift 


m 


m 


10 


»o « 




i-g 




GO 


%o 


rh 




<7\ 


»-l c^ 






















•0 

0) 




Red 

tion 
are 


P^ 





CO 


r- 




1-1 


"t^ 
























' ^ f> 




>o 


m 














4) 




ecu 


■s 


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ti 


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*H 








00a 


(k 
















» 




W-N 




















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^ 












































C7t 


ca 


o\ 


c^ t> 






% 


on 


CO 


h* 


CM 


fN, 


r-* r^ 
























ti-s 


Hi 




CO 


CO 


CM 




CM CM 






q* 





<-> 


(-> 




r> 










































rH 








































SS 


S 


5S 

CM 


CO 

c>a 


C7* 

CNJ 




s 








Propor- 
tional 
limit 


q- 









































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1-1 








y-A 




y-K i-« 








1 




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r* 


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on 


t>. 




ta 
















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1 




a 

3 

n 


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m 


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o\ t-- 








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o> 


CM 


CO 


CM 


CO CM 




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Red 

tion 

are 




CO 


r- 


00 


Th 


Th 




rf 


•0 

N 




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rj 




CO 


T-l 


■«3- 








adS 



















10 




long 
oni 
inch 








i4 


CM 


^ 


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d 





r> 


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r^ 




























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n 




n 












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m 


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p 




















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a 




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tf 


H 




































3 

a 

i 





< 


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d 






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Ti4 








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ift 




K 


in 




CM 


CM 


C^J 


CM CnS 




e 


•g 


\o 


-^^ 


CM 


CO 


00 


s g 






s 




r^ 


00 






r^ 






& 


c5 


• 




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• 


1-1 






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m 


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m CO 






w 


p: 


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CO 


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10 in 








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• 




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' 


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d 














iM o\ 












1-1 


r4 w< 


CM 


§ ft 


K 

•« 


• I 



Burgess T 
Woodwards 



Zirconium Steels 



165 



4> 
4> 

CO 

§ 

In 
O 

0) 






s 
o 

In 

O 
I 



s 



1 

CB 
4) 

i 


1 


w t-- 00 *0 
Q CO ■«■ CO 


1 = 

fi 


ii 


CO C^J 
CO ■<4- to 


1 

PQ 


c* «o I>- 

.-H Irt CO 
N Xft CO 


•ocg 
«J.sS 


. 1-1 00 c^ 


Elonga- 
tion in 2 
inches 


. 0^ lA 1-t 
" CO ■ ■ 

pI 


is 


Lbs./in.» 
96 100 

150 000 
85 400 


2-3 


— • ^ 

ffl : c~ : 

iJ : -^ ; 


1 

111 


■S g ° • 
a S » • 


1 

1 




ii 




2 i S 


a 

n 


S S £ 

•-( r4 rH 


•§a£ 
PS- 


_^ 00 t^ 
u (Tj ui -J 

• N CM -^ 


Elonga- 
tion in 2 
inches 


^ r^ m 
" d -• C-- 

p; - - - 


"fi 

a <3 

5^ 


a § s s 

^ 00 vo m 

2 o\ ■<^ 

.Q to 07 


P 


Lbs./in.a 

46 300 
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(s;s= 


nisi 


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1 
U 


m 


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< 


■s g g g 

ft ■ ■ 


a 


t> J ; ; 

ft : ■ : 



S 


tS 00 C7\ 
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pI d • • 


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P< d -^ 





■?3 to »-< m 
'^ ^ CM -a- 

0< d ■ ■ 




i 




B S S 

ra CM *>a 

VH t-l *H 



r>. o !>■ o »n o 



t^ 





o^ 


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ti-> 


N 


M 


10 


c* 


t> 


c^ 


00 


ca 


CO 


eo 








d 


CO 


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CM 


CO 


CO 



000000 
000000 
C3\ CO m t^ CO *-< 

o 00 ^- VO vo to 
t^ O *-< (Nj tr> fj 
f-H eva oa eg c«3 CO 



000 



rH csa c^ 



000000 
000000 
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^- ra CO »n o O 

,_, ^ ,-( en O C-- 



O o in in ra to 
oa a^ c^ o vo 00 
rg ^ ^ t>a c^ (va 



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00 


00 


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m o 00 o o o 
d ^ d cvi c-^ *-5 



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o in o o o o\ 

1-" \D 0^ vO CM CO 



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CO 


m 

























, 






^ 








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in 


vn 

















m 




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CO 


CO 


CO 


CO 


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<£> 


m 


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in 



















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r-« 























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m 








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i66 



Technologic Papers of the Bureau of Standards ivoi. r6 



3 

a 

JO 



o 

1-4 

o 






Q 

n 

O 

O 









Cl 


00 




N 








u 


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c^ 






A 


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a 


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CO vo en 








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■ga 

09 9 


ig" 














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CM tt o> 00 




a 




to <«• CO xo to 






■n 
















n 












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IP 


p; 


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00 tn m 00 1 







t^ Vi^ lO "o^ i> 1 




o a u 


p; 










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d 






at 






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a 












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h) 


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■o-s 


e 







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CO 




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, 


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c 





















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n; 




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strength 


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5 
















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p; 








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d 






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g 


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ra 




a 

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CO 


CO CO 


a 


ts 


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s 


cr 


oc 


oc 






p^ 


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• 




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to 





00 t£> 




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to CO CM 

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00 >0 CO 

f-H CQ (M 











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d 


CM 










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CO 









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d 


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d 




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CO 

d 


CO 


to 



Burgess I 
Wood-ward] 



Zirconium Steels 



167 






CO 



I 

o 

A! 
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r 


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in 




1 


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in 

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ca 


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CM 








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in 


c^ 


10 


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a> 0^ 
















il 


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in 


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C^ 


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w« 


a 

n 




m 


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vC 


m 


m 


t ^ 




m 


CO 


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to 


eo 




ii ® c8 
















5g2 





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to 


d 




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ca 


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ra 


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f 

w- 


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r-5 






a 






















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m 


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Cs] 




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10 


00 





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i 


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p; 


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1 68 



Technologic Papers of the Bureau of Standards [Voi.16 











04 




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ro 


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fe 




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« 


Elon- 
gation 
in2 
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u 


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CO 

in eg 






cu 


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u 
































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Burgess I 
Wood-wardJ 



Zirconium Steels 



169 



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1 70 Technologic Papers of the Bureau of Standards . Woi. 16 

VII. SUMMARY AND CONCLUSION 

1. About 193 heats of steel, containing in various combinations 
the principal variable elements of carbon, silicon, nickel, aluminum, 
titanium, zirconium, cerium, boron, copper, cobalt, uranium, 
molybdenum, chromium, and tungsten, have been studied. 

2. None of the steels presented any difficulties in rolling into 
plate except those containing boron. 

3. The usual mechanical and impact tests were carried out on 
all of the steels. It is shown that steel containing 0.40 to 50 
per cent carbon, i to 1.50 per cent silicon, 3 to 3.25 per cent 
nickel, and 0.60 to 0.80 manganese and deoxidized with a simple 
deoxidizer such as alumium can be produced having a tensile 
strength of approximately 300 000 lbs. /in. ^ with excellent ductility 
and toughness. This type of steel is recommended for structural 
material. 

4. Although the same high properties are obtained in steels of 
the above composition with the aid of additional elements, it does 
not appear necessary to resort to such additions of more costly 
alloying elements. 

5. Zirconium, like titanium and aluminum, acts primarily as a 
scavenger, and when it is not removed as part of the slag remains 
in the steel in the form of square bright-yellow inclusions not 
directly visible at magnifications lower than 500 x - It is not con- 
sidered that these inclusions can be very beneficial, and if they are 
segregated into groups and rolled out into thin platelike streaks 
they may be detrimental. 

6. Of the other elements that are regarded as special alloying 
additions, chromium, tungsten, vanadium, and molybdenum go 
into solution and produce a martensitic pattern in the air-cooled 
specimens. Cerium and uranium act in a similar manner, but also 
show characteristic inclusions. Copper goes into solution, but a 
larger amount is required to produce a martensitic pattern in the 
air-cooled samples than for the others. Boron forms a complex 
eutectic, probably that of an iron-carbon-boron compound with 
iron. This eutectic is fusible at the temperatures ordinarily used 
in rolling, but at slightly lower temperatures steel containing 
boron can be rolled successfully. Hot working breaks up the 
eutectic, and spherical hard particles, similar to iron carbide 
globules, are formed. 



woodward] Zirconium Steels 171 

Vm. ACKNOWLEDGMENTS 

An investigation covering so many fields of work required the 
cooperation of many individuals. The authors consider that any 
merits the investigation may possess are largely due to their collab- 
orators. 

The development of the methods of chemical analysis was the 
contribution of Dr. G. E. F. Lundell, who, assisted by H. B. 
Knowles and part time by Ensign R. McLane, J. R. Eckman, and 
Miss E. R. Ward, also made the chemical analyses for the unusual 
elements. The rolling of the plates was mainly carried out by 
R. G. Waltenberg, assisted by R. D. France and W. M. Laughton. 
The last and F. C. Speidel assisted in determining the mechanical 
properties. Most of the heat treatment was done by H. R. Yerger 
and the microexaminations entirely by S. Epstein, and H. Scott 
was responsible for most of the results in thermal analysis. 

Washington, March 30, 1921. 



APPENDIX 

THE DETERMINATION OF ZIRCONIUM IN STEEL » 

By G. E. F. Lundell and H. B. Knowles 

(a) PRELIMINARY STATEMENT 

The method developed at the Bureau of Standards permits the determination of 
silicon, altmiinum, titanium, and zirconium in one portion of the steel and provides 
for the following possible interfering elements: Tungsten, chromium, uranium, 
cerium, manganese, phosphorus, vanadium, molybdenum, copper, nickel, and 
cobalt. 

(b) METHOD 

Dissolve 5.00 g of the steel in 50 cc of hydrochloric acid (sp. gr. 1.2) with gentle 
warming and the addition of one cc portion of nitric acid from time to time to insure 
solution of the zirconium and titanium and also oxidation of the iron. 

When solution is complete, evaporate to dryness, take up in 10 cc of hydrochloric 
acid (sp. gr. 1.2), again evaporate to dryness, and finally bake at a gentle heat in order 
to decompose nitrates. Cool, take up in 50 ccof i :i hydrochloric acid, and filter 
when the iron is completely in solution. Wash the residue with hot 3 per cent hydro- 
chloric acid. Save the filtrate and washings. 

Ignite the residue and paper in a platinum crucible, cool, and weigh. Treat 
with I cc of sulfuric acid (1:1) and suflScient hydrofluoric acid, fume off in the usual 
manner, ignite and weigh to obtain silica, and calculate silicon. Fuse the slight 
residue left after the hydrofluoric acid treatment with a small amotmt of potassium 
pyrosulfate, dissolve in 10 to 20 cc of 5 per cent sulfuric acid and add the solution 
to the acid extract from the ether separation obtained as described below. 

Evaporate the filtrate and washings from the silica determination to a sirupy con- 
sistency, take up in 40 cc of hydrochloric acid (sp. gr. i.i) and extract with ether in 
the usual manner. (The ether extract will contain most of the molybdenum, and this 
element may be qualitatively tested for in it. If molybdenum is present, it is more 
conveniently determined in a separate portion of steel. ) The acid extract will contain 
some iron and all of the zirconium, titanium, aluminum, nickel, chromium, etc. 

Gently boil off the ether in the acid extract, add the matter recovered from the silica, 
oxidize ferrous iron with a little nitric acid, dilute to 300 cc, cool, and precipitate 
with 20 per cent sodium hydroxide solution, adding 10 cc in excess. The sodium, 
hydroxide solution should be as piu-e as possible and free from carbonate. Filter 
and save the filtrate. Dissolve the precipitate in warm dilute i : i hydrochloric acid, 
repeat the sodium hydroxide precipitation, filter, and combine the sodium hydroxide 
filtrates. Dissolve the sodium hydroxide precipitate in warm dilute i : i hydrochloric 
acid and reserve the solution for subsequent analysis. 

It is advisable to treat as follows the filter or filters used above : Ignite in platinum, 
fuse with sodium carbonate, digest the cooled melt with hot water, wash the residue, 
discard the filtrate and washings, dissolve the residue in hot i : i hydrochloric acid, and 
add to the main acid solution. This precaution makes certain the recovery of any 
zirconium held back on the filter as zirconium phosphate insoluble in acid. 

I J. Ind. and Eng. Chem., 12, p. 563; 1920. 
172 



wcoZ'ord] Zirconium Steels 173 

Determination of Aluminum 

(o) In the absence of chromium and uranium add a few drops of methyl red to the 
sodium hydroxide filtrate, neutralize with hydrochloric acid, add 4 cc of concentrated 
hydrochloric acid per 100 cc of solution, boil, make barely alkaline with ammonium 
hydroxide, continue the boiling for 3 minutes and set the beaker aside for 10 minutes. 
If no precipitate settles out, the absence of aluminum is assured. If a white precipi- 
tate settles out, aluminum is indicated. This precipitate is always contaminated by 
phosphorus pentoxide and must be purified as follows: Filter without washing, dis- 
card the filtrate, and dissolve the precipitate in warm i : i hydrochloric acid. Dilute 
the solution to 50 cc, make alkaline with ammonium hydroxide, neutralize with nitric 
acid, and add 2 cc in excess. Warm to 50° C, precipitate the phosphoric acid with 
molybdate reagent in the usual manner, filter, and wash the phosphomolybdate with 
an ammonium acid sulfate solution. Precipitate the alumintun in the filtrate as 
directed above, filter without washing, dissolve the precipitate in warm i: r hydro- 
chloric acid, reprecipitate, filter, wash slightly with 2 per cent ammonium chloride 
solution, and ignite in a platinum crucible. The ignited residue is usually contami- 
nated by silica. Therefore a sulfuric acid-hydrofliiroic acid treatment, followed by 
ignition to alumina over the blast lamp, should be performed. (The sodium hydroxide 
reagent must be tested for substances precipitable by ammonia, and appropriate 
corrections must be made in the aluminum determination when these are present.) 

{b) In steels containing chromium proceed as above until the filtrate from the 
molybdate precipitation is obtained. Then make the solution ammoniacal, oxidize 
with a little bromine water, make just acid with 1:2 nitric acid; add ammonium 
hydroxide in slight excess, heat to boiling, filter, dissolve the precipitate in dilute 
hydrochloric acid, and reprecipitate the alumintmi hydroxide as directed above. 

(c) In steels containing uranium the only modification which is reqmred is the 
substitution of ammonium carbonate for ammonium hydroxide as the final precipi- 
tant of the aluminum hydroxide. 

(d) In steels containing vanadium, "alumina which is obtained by the above pro- 
cediires from steels containing vanadium is contaminated by this element. When 
dealing with these steels, proceed as follows: Fuse the weighed residue with pyro- 
sulfate, extract the cooled melt with 5 per cent sulfuric acid, reduce the vanadium in 
a Jones reductor having ferric alum in the receiver, titrate the reduced solution with 
standard permanganate, calculate the vanaditun as V^O^, and subtract from the 
original weight. 

Deteimination of Zirconium and Titanium 

Dilute the hydrochloric acid solution to 250 cc, neutralize with ammonium hydrox- 
ide, so as to leave approximately 5 per cent (by volume) of hydrochloric acid, add 2 g 
of tartaric acid , and treat with hydrogen sulfide until the iron has been reduced . Filter 
if the sulfide group is indicated. Make the hydrogen sulfide solution ammoniacal 
and continue the addition of the gas for five minutes. Filter carefully and wash with 
dilute ammonium sulfide-ammonium chloride solution. Filter through a new filter 
if the presence of iron sulfide in the filtrate is indicated. Save the filtrate. (The 
sulfide precipitate consists of ferrous sulfide in addition to the greater part of ihy 
nickel, cobalt, and manganese present in steel. It is preferable to determine these in 
separate portions of the steel.) 

Neutralize the ammonium sulfide filtrate with sulftiric acid, add 30 cc in excess, 
and dilute with water to 300 cc. Digest on the steam bath imtil sulfiy and stdfides 
have coagulated, filter, wash with 100 cc of 10 per cent sulfuric acid, and cool the 
filtrate in ice water. Add slowly and with stirring an excess of a cold 6 per cent water 
solution of cupferron. (The presence of an excess is shown by the appearance of a 
white cloud, which disappears, instead of a permanent coagulated precipitate.) After 
10 minutes filter on paper, using a cone and very gentle suction, and wash the pre- 



174 Technologic Papers of the Bureau of Standards [Voi.i6 

cipitate thoroughly with cold lo per cent hydrochloric acid. Carefully ignite in a 
tared platinum crucible, completing the ignition over a blast lamp or large Meker 
burner, cool, and weigh the combined zirconinum and titanium oxides. Fuse with 
potassium pyrosulfate, dissolve in 50 cc of 10 per cent (by volume) sulfinic acid, and 
determine titanium colorimetrically or volumetrically. Calculate titanium oxide, 
subtract the weight found from that of the combined oxides, and calculate zirconium, 

(c) NOTES ON THIS METHOD 

1. Phosphorous pentoxide contaminates the precipitate to so slight an extent that 
it can be disregarded. 

2. Vanadium interferes no matter what its valency. The interference is not quan- 
titative. If present in the steel, proceed as usual through the weighing of the cup- 
ferron precipitate. Then fuse thoroughly with sodium carbonate, cool, extract with 
water, filter, and determine the vanadium in the filtrate by adding sulfiuric acid, 
reducing through a Jones reductor into a solution of ferric alum-phosphoric acid and 
then titrating with standard permanganate. Vanadium is thus reduced to V2O2 and 
then oxidized to V2O5. Calculate V2O5 and subtract from the combined oxides. 
Ignite in the original crucible the matter insoluble in water, fuse with potassium 
pyrosulfate and proceed as directed for titanium. 

3. Tungsten does not interfere, since it is separated from zirconium and titanium by 
the sodium hydroxide treatment and from aluminum by the ammonixmi hydroxide 
precipitation. If tungsten is present in large amount it may be found desirable to fuse 
the nonvolatile residue from the silicon determination with sodium carbonate, extract 
with water, filter, dissolve the residue in hot 1:1 hydrochloric acid, and add to the 
acid extract from the ether separation. 

4. Uranium is partially carried down when present in the quadrivalent condition, 
but not at all in the sexivalent state. If this element is suspected, boil out all hydro- 
gen sulfide before the cupferron precipitation, oxidize with permanganate to a faint 
pink, cool, and proceed with the cupferron precipitation. 

5. Thorium and cerium interfere, but they are not thrown down quantitatively. In 
case these elements are suspected the peroxidized solution used for the titanium deter- 
mination must be quantitatively preserved and reduced with a little sulfurous acid. 
The rare earths are then separated by Hillebrand method,^ as follows: Precipitate the 
hydroxides with an excess of potassium hydroxide, decant the liquid, wash with water 
once or twice by decantation, and then slightly on the filter. Wash the precipitate 
from the paper into a small platinum dish, treat with hydrofluoric acid, and evaporate 
nearly to dryness. Take up in 5 cc of 5 per cent (by volume) hydrofluoric acid. If no 
precipitate is visible, rare earths are absent. If a precipitate is present, collect it on a 
small filter held by a perforated platinum or rubber cone and wash it with from 5 to 
10 cc. of the same acid. Wash the crude rare-earth fluorides into a small platinum 
dish, bum the paper in platinum, add the ash to the fluorides, and evaporate to dry- 
ness with a little sulfuric acid. Dissolve the sulfates in dilute hydrochloric acid, 
precipitate the rare-earth hydroxides by ammonia, filter, redissolve in hydrochloric 
acid, evaporate the solution to dryness, and treat the residue with 5 cc of boiling hot 
5 per cent oxalic acid. Filter after 15 minutes, collect the oxalates on a small filter, 
wash with not more than 20 cc of cold 5 per cent oxalic acid, ignite, and weigh as rare- 
earth oxides which are to be deducted from the weight of the cupferron precipitate. 

The above procedm'e does not give an absolutely quantitative recovery of the rare 
earths. Experiments indicate a recovery of approximately 85 per cent of the rare 
earths present in residues containing 100 mg of zirconia, 2 mg of thoria, and a mg of 
ceria. Attempts which were made to omit the preliminary separation of the rare 
earths, as fluorides, were imsuccessful. 

a U. S. Geol. Survey, Bui. 700. p. 176. 



Burgess T 
Woodward] 



Zirconium Steels 



175 



6. Instead of the prescribed treatment for the removal of the bulk of the iron, 
Johnson's ^ method of fractional precipitation with ammonium hydroxide may be 
used. When using this method, it is recommended that the i : i hydrochloric acid 
solution of the ammonium hydroxide precipitate should be further treated as given 
in the Bureau of Standards method beginning with "oxidize * * * and precipi- 
tate with a 20 per cent sodium hydroxide solution. " In Johnson's procedtu-e silicon 
must be determined in a separate portion. 

7. After considering the method and studying the notes the reader might ask the 
question, "Why not use ammonium hydroxide instead of cupferron as the final pre- 
cipitant?" The disadvantages of such a procedure are the following: (o) The neces- 
sity for destroying the tartaric acid which is in the solution, with attendant danger 
of contamination by material resulting from the attack on glassware; {b) the copre- 
cipitation of phosphorus and also chromium and uranium when they are present. 

The advantages of an ammonia precipitation are: (a) It is a cheaper reagent; (6) the 
precipitation of cerium would be complete instead of partial. 

The following scheme of analysis is now being tested at this Bureau: Zirconium, 
titanium, aluminum, cerium, chromium, vanadium, etc., are first separated from the 
bulk of the iron by Johnson's method, and the hydrochloric acid solution of this pre- 
cipitate is then treated with sodium hydroxide and sodium peroxide as described by 
Noyes, Bray, and Spear.'' It is hoped that this treatment will quantitatively precip- 
itate iron, zirconium, titanitun, and cerium, leaving such elements as aluminum 
uranium, vanadium, chromium, tungsten, molybdenum, and phosphorus in solution. 
Iron, manganese, and the greater part of the copper, nickel, and cobalt are next sepa- 
rated by precipitation with ammonium sulfide in the presence of tartrate, as recom- 
mended by Thornton,* and zirconium, titanium (and cerium) are finally precipitated 
by ammonia after destroying the tartaric acid. The ignited and weighed precipitate 
is then treated for titanium and the rare earths as described in the Bureau method. 

(d) CONFIRMATORY EXPERIMENTS 

Below is given a summary of the data obtained in the analysis of the Biueau of 
Standards acid-open-hearth steel No. 20a to which definite amounts of standardized 
solutions were added. 



Mo. 


V 

present 

G 


Cr 

present 
G 


Cu 

present 
G 


Nl 

present 

G 


Al 

added 
G 


Al 

found 

G 


T 

added 
G 


Ti 

found 

G 


Zr 

added 

G 


Zr 

found 
G 


1 


0.0005 


0.0009 


0.0034 


0.0009 


None 


None 


None 


None 


None 


None 


2 


.0005 


.0009 


.0034 


.0009 


None 


None 


None 


None 


None 


None 


3 


.0005 


.0009 


.0034 


.0009 


0. 0100 


0.0101 


0.0100 


a 0.0102 


0. 0101 


6 0. 0097 


4 


.0005 


.0009 


.0034 


.0009 


.0100 


.0094 


.0100 


0. 0102 


.0101 


6.0097 


5 


.0005 


.0009 


.0034 


.0009 


.0500 


.0502 


.0476 


C.0482 


.0500 


6. 0493 


6 


.0005 


.0009 


.0004 


.0009 


.0500 


.0501 


.0476 


C.0482 


.0500 


6.0492 



o Colorimetrically . 

6 The special treatment for vanadium (see note 2) was not carried out. This furnishes an interesting 
light on the slightly higher values for titanium obtained both colorimetrically and volumetrically and 
the correspondingly lower values for zirconium which resulted on account of the omission of this step. 

c Volumetrically after reduction in a Jones reductor and collection in ferric-alum solution. 



• Loc. cit. 

* Technology Quarterly, 21, p. 35, 1908. 
' Am. J. Sci., 87, p. 173, 1914. 



176 Technologic Papers of the Bureau of Standards [Voi.16 

The following modifications of the above method were employed by Lieut. R. 
McLane in the analysis of zirconium steels at the Ithaca station of the Bureau of 
Mines: 

1. Treat the evaporated solution containing silica with 25 cc of hydrochloric acid 
(sp. gr. 1.2), again evaporate to dryness, bake and take up in 30 cc of hydrochloric 
acid (sp. gr. i. 2)4-40 cc of water. 

2. Ignite the insoluble residue and without weighing (silica being obtained on a 
separate sample by dehydration with sulphuric acid) add 2 cc of sulphuric acid (sp. 
gr. 1.84), an excess of hydrofluoric acid, and fume off the sulphuric acid. Dissolve 
the unignited residue in hydrochloric acid (i : i) and add to the acid extract from 
the ether separation. 

3. Evaporate the filtrate from the silica determination to 25-40 cc volume, cool by 
placing in a larger beaker through which a stream of water is passed, and add 200 cc 
of ether. Stir, let settle, decant off ether, add 100 cc more ether, and repeat the 
operation. Perform a third extraction, if necessary, and pipette off the last of the 
ether, thus avoiding any transfer of the solution. 

4. To separate aluminum, heat the oxidized solution to boiling and pour it with 
constant stirring into 135 cc of hot sodium hydroxide solution (20 per cent) contained 
in a 600 cc Pyrex beaker. After the precipitate has settled filter, allow the filtrate 
to stand overnight, and refilter if a precipitate appears. One extraction carried on 
as above is sufficient. 

5. Place the filters and precipitates in the original beaker, add 25 cc of hydrochloric 
acid (sp. gr. 1.2), dilute to 125 cc, and heat. Filter off the insoluble, wash, ignite, 
fuse with sodium carbonate, and proceed as in the method. 

6. Add methyl red and 8 cc of ammonia (sp. gr. 0.9) to the sodium-hydroxide fil- 
trate, make slightly acid with hydrochloric acid, dilute to 500 cc, heat to boiling, and 
make just alkaline with ammonia. Let stand warm for one hour, filter, dissolve the 
precipitate in hydrochloric acid, and dilute the cooled solution to 100 cc volume. 
Take out exactly 10 cc for a FejOg determination by the colorimetric thiocyanate 
method. Precipitate the remainder of the solution as above and proceed with the 
molybdate separation as in the method. Finally deduct nine-tenths of the blank 
(blank has had SiO^ and FejOj deducted and is usually negligible) and divide the 
weight of AI2O3 by 0.9, giving AI2O3. 

7. Treat the ignited cupferron precipitate with an excess of sulphuric and hydro- 
fluoric acids, evaporate, ignite, and weigh in order to correct for any silica present. 

8. Dissolve the weighed precipitate in sulphuric and hydrofluoric acids, evaporate 
to fumes of sulphuric acid, and make up to definite volume. Determine TiOj in one 
aliquot portion by the colorimetric peroxide method and FcjOs in another by the 
colorimetric thiocyanate method and deduct. 

The authors desire to express their thanks to Dr. W. F. Hillebrand for valuable 
suggestions and advice. 



